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Microwave synthesis of JWH-018

William Dampier

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Reaction scheme:
NZ1iBTbJUl

Synthesis:
1. Indole (0,117 g) was mixed with neutral Al2O3 (1 g) and ground together until a homogeneous powder was formed.
2. 1-naphthoyl chloride (0,286 g) was added to the mixture and stirred to homogeneity.
3. The final mixture in a sealed 5 ml microwave vial was subjected to irradiation in a microwave reactor at 100 *C (400 W) for 8 minutes.
4. After cooling to room temperature, 0,16 g of Na2CO3 as a finely ground powder and 0,18 g of 1-bromo-pentane were added into the microwave vial and then stirred to homogeneity.
5. The resulting mixture was irradiated again in the microwave reactor at 100*C (400W) for 4 minutes.
6. Then, 60 ml EtOH was added to the reaction mixture and refluxed for 20 minutes.
7. Al2O3 was filtered and washed with 15 ml water twice, and dried for a next cycle.
8. The EtOH phase was treated with a solution of 10 ml water, after which a solid was formed.
 
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jexana23

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I m a novice , can you explainbetter, i search for indole and i found many tipes of indole and my brain go down :)
How much quantyti etc.
 
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jexana23

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Reaction scheme:
View attachment 1666
Synthesis:
1. Indole (0,117 g) was mixed with neutral Al2O3 (1 g) and ground together until a homogeneous powder was formed.
2. 1-naphthoyl chloride (0,286 g) was added to the mixture and stirred to homogeneity.
3. The final mixture in a sealed 5 ml microwave vial was subjected to irradiation in a microwave reactor at 100 *C (400 W) for 8 minutes.
4. After cooling to room temperature, 0,16 g of Na2CO3 as a finely ground powder and 0,18 g of 1-bromo-pentane were added into the microwave vial and then stirred to homogeneity.
5. The resulting mixture was irradiated again in the microwave reactor at 100*C (400W) for 4 minutes.
6. Then, 60 ml EtOH was added to the reaction mixture and refluxed for 20 minutes.
7. Al2O3 was filtered and washed with 15 ml water twice, and dried for a next cycle.
8. The EtOH phase was treated with a solution of 10 ml water, after which a solid was formed.
Can you explain for stupit noob people like me , i know i m very stupid but if you explain for noobs i think it a possible to understand
 

HEISENBERG

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I m a novice , can you explainbetter, i search for indole and i found many tipes of indole and my brain go down :)
How much quantyti etc.
CAS 120-72-9
 

nutritiousforeach

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Reaction scheme:
View attachment 1666
Synthesis:
1. Indole (0,117 g) was mixed with neutral Al2O3 (1 g) and ground together until a homogeneous powder was formed.
2. 1-naphthoyl chloride (0,286 g) was added to the mixture and stirred to homogeneity.
3. The final mixture in a sealed 5 ml microwave vial was subjected to irradiation in a microwave reactor at 100 *C (400 W) for 8 minutes.
4. After cooling to room temperature, 0,16 g of Na2CO3 as a finely ground powder and 0,18 g of 1-bromo-pentane were added into the microwave vial and then stirred to homogeneity.
5. The resulting mixture was irradiated again in the microwave reactor at 100*C (400W) for 4 minutes.
6. Then, 60 ml EtOH was added to the reaction mixture and refluxed for 20 minutes.
7. Al2O3 was filtered and washed with 15 ml water twice, and dried for a next cycle.
8. The EtOH phase was treated with a solution of 10 ml water, after which a solid was formed.

Why is irradiation specifically used, instead of normal controlled heating at 100*C? Just wanted to understand the chemistry. Thank you.
 

krtl91

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hi there . thank you for information. what can i use instead of 1 naphtoyl chloride ? i cant find it commercially here . or how can i make for my self ? thx
 

William Dampier

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hi there . thank you for information. what can i use instead of 1 naphtoyl chloride ? i cant find it commercially here . or how can i make for my self ? thx
1-naphthoyl chloride substituted - 4-methoxy or 4-ethyl -1-naphthoyl chlorides. 1-Adamantanecarbonyl chloride, 2-Iodobenzoyl chloride, 2,2,3,3-Tetramethylcyclopropanecarbonyl chloride, etc
 

krtl91

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is there one which i could find commercially available easier than others ? thank you
 

krtl91

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1-naphthoyl chloride substituted - 4-methoxy or 4-ethyl -1-naphthoyl chlorides. 1-Adamantanecarbonyl chloride, 2-Iodobenzoyl chloride, 2,2,3,3-Tetramethylcyclopropanecarbonyl chloride, etc
hi there .Thank you for your time . İ am having trouble to find those reagents commercially available. Which one of those i can synthesis myself from the commercially available ones (as a amateur one i would prefer to easiest one ) thank you :) .
 

William Dampier

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You can find acid, not chloride (for example naphthoyl acid) and make chloride with thionyl chloride or phosphoryl chloride. Synthesis (click). You can use other acids, by analogy.
 

krtl91

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You can find acid, not chloride (for example naphthoyl acid) and make chloride with thionyl chloride or phosphoryl chloride. Synthesis (click). You can use other acids, by analogy.
none of them İ mean literally none of them available commercially in my frkng country. ı guess ı ll just order napthoyl cloride from chına or somewhere and do the procedure . coz ı assume as a amateur ıt doesnt worth to that much trouble to optaın naphtoyl chlorıde when ıts avaılable commercially ın other countrıes
 

William Dampier

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Yes, of course it is better to buy chloride than to make it, not the most pleasant procedure.
 

northenos

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What equipment needed to microwave synthesis ?
 

William Dampier

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MW oven, beakers, scales, grinders, filters, etc.
PS: Who synthesizes ADBB-noids with main reagent (with potassium carbonate), can try this synthesis starting from step 4
 

northenos

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I still confused start step 6, what equipment needed to reflux ?
any video to explain that ?
 

northenos

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After reflux, the mixture filtered and the filter washed with water twice ? How to wash that i need example, and step 8 i still confused with the word “EtOH phase”, what is EtOH phase ?
 
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