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William D.

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Reagents:
  • Indole (cas 120-72-9) 1000 g;
  • Dichloromethane (CH2Cl2) 15 l;
  • Tin(IV) chloride (SnCl4) 2000 ml;
  • 1-Naphthoyl chloride (cas 879-18-5) 1627 g;
  • Nitromethane (cas 75-52-5) 10 l;
  • Distilled water 20 l;
  • Ethyl acetate (EtOAc) 15 l;
  • Sodium or magnesium sulphate (Na2SO4 or MgSO4);
Equipment and glassware:
  • Batch reactor 50 l with a top stirrer;
  • Ice bath;
  • Vacuum source;
  • Rotovap machine;
  • Several buckets;
  • Laboratory scale (1-1000 g is suitable);
  • Funnel;
  • Glass rod and spatula;
  • Pyrex dish;
Reaction scheme:
4Wkp2TNLYR
Synthesis:
1. Tin(IV) chloride (SnCl4) 2000 ml is added in a single portion to an indole 1000 g solution in dichloromethane (CH2Cl2) 15 l in a batch reactor 50 l.
2. The mixture is stirred at room temperature for 30 min after an ice bath was removed. Then 1-naphthoyl chloride 1627 g is added to the reaction suspension in small portions, followed by nitromethane 10 l.
3. Then, the mixture is stirred for 2 h at room temperature.
4. Next, the reaction mixture is quenched with an ice cold water 20 l. The mixture is filtered in order to remove inorganic precipitates. Layers are separated.
5. The water layer is
extracted with ethyl acetate (EtOAc) 15 l. EtOAc extract is combined with organic layer.
6. The organic phase is
dried over sodium or magnesium sulphate (Na2SO4 or MgSO4) and concentrated at reduced pressure. A crystalline solid 3-(1-Naphthoyl)indole product (cas 109555-87-5) is obtained.

 
Last edited by a moderator:

ASheSChem

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it is possible to obtain SnCl4 with SnCL2.2H2O?
 

ASheSChem

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4. After being quenched with ice and water (20 liters), the mixture was filtered to remove inorganic precipitates, and the organic material was extracted with ethyl acetate (15 liters).
William Dampierso; we put water and ice in the mixture, we filter all the mixture; we add ethyl acetate and after separate 2 layers?

The organic phase was dried over Na2SO4 and concentrated at reduced pressure to give the product as a crystalline solid.
so... we put Na2SO4 in the ethyl acetate ? (how much Na2SO4?) and... i don't realy understand what to do.. evaporte, distill, filter.. i am lost :p
 

G.Patton

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I got this after ethyl acetate extraction. its oily and sticky and doesnt dry to form crystals, what was my mistake?

View attachment 5041
madmoney69Are you sure in all your reagents? Have you checked melting points of them? It's happens by reason of bad reagents (spoiled, out of exp date, wet) quite often in organic synthesis.
 

William D.

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There may be different reasons. When we do, we will publish it here.
 

Techtrain

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Questions:
. To a stirring solution of indole (1000 g) in CH2Cl2(15 liters) was added SnCl4(2000 ml) in a single portion.
2. After the ice bath was removed.

To a stirring solution: does the stirring speed matter? Or this is just hand stirring at normal rate?

After the ice bath was removed?

So start with ice bath to begin step 1 stirring solution?
 

Techtrain

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Are you sure in all your reagents? Have you checked melting points of them? It's happens by reason of bad reagents (spoiled, out of exp date, wet) quite often in organic synthesis.
G.Patton How are melting points checked?
And exp dates?
 

Selassi

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I got this after ethyl acetate extraction. its oily and sticky and doesnt dry to form crystals, what was my mistake?

View attachment 5041
madmoney69Swim too is familiar with this problem, doest seem.to crystallize. Even after trying to recryss, it keeps coming out thick and oily.
It is active as fk though...
 

William D.

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Swim too is familiar with this problem, doest seem.to crystallize. Even after trying to recryss, it keeps coming out thick and oily.
It is active as fk though...
SelassiMany have difficulty with this synthesis. I would advise starting with pentylindole, there will be less excess polymerization.
 

Gusto4205

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Best way to filter?
 

Gusto4205

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D
so; we put water and ice in the mixture, we filter all the mixture; we add ethyl acetate and after separate 2 layers?


so... we put Na2SO4 in the ethyl acetate ? (how much Na2SO4?) and... i don't realy understand what to do.. evaporte, distill, filter.. i am lost
ASheSChemDid you get a answer to this question?
 

charmingcho

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When I experimented, the solution became dark chocolate color when I added naphthonyl chloride.

Then, two hours later, ice and water were added to the solution to produce a light brown insoluble precipitate.

Then I added ethyl acetate to the solution, and the ethyl acetate layer was on top of it, and the color of the solution was chocolate. And the solvent was evaporate, but it remained an equally sticky dark brown liquid.
 
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