SGT-263 (CUMYL-5F-P7AICA)

[William D.]

Reaction scheme:

Synthesis:
1. A solution of 1H-pyrrolo[2, 3-b]pyridine-3-carboxylic acid (0.49 g, 3 mmol), oxalyl chloride (0.6 mL, 7.2 mmol), and DMF (1 mL) in dichloromethane (20 mL) was stirred for 20 min.
2. The mixture was evaporated and then redissolved in methanol (20 mL) and stirred for 40 min.
3. The mixture was evaporated and then extracted with ethyl acetate.
4. The organic phase was washed with saturated sodium bicarbonate solution and dried with Na2SO4, and the solvent was removed in vacuo to yield the white solid (0.36 g, 68%).
5. A solution of Step 4 (0.36 g, 2 mmol), potassium t-butoxide (0.27 g, 2.4 mmol), and 1-bromo-5-fluoropentane (1.6 g,9.5 mmol) in THF (20 mL) was stirred for 24 h.
6. The mixture was extracted with ethyl acetate.
7. The organic phase was washed with brine and dried with Na2SO4, and the solvent was removed in vacuo.
8. The residue was purified by silica gel chromatography with stepwise gradient elution of n-hexane/ethyl acetate (3:1–2:1–1:1, v/v) to yield the white solid (0.35 g, 65%).
9. A solution of step 8 (0.35 g, 1.3 mmol) and 6 mol/L sodium hydroxide solution (10 mL) in methanol/THF (2:1,v/v, 15 mL) was stirred for 1.5 days.
10. The mixture was evaporated, added to water, and then washed with ethyl acetate.
11. A solution of 1 mol/L hydrochloric acid was added to the aqueous phase, and the mixture was extracted with ethyl acetate.
12. The organic phase was washed with brine and dried with Na2SO4, and the solvent was removed in vacuo to yield the white solid (0.39 g, quant.)
13. A solution of step 12 (0.39 g, 1.3 mmol), oxalyl chloride (3 mmol), and DMF (1 mL) in dichloromethane (12 mL) was stirred for 10 min.
14. The mixture was evaporated and then redissolved in dichloromethane (10 mL).
15. Cumylamine (2 mmol) and triethylamine (0.5 mL) were added to the solution and stirred for 15 h.
16. The mixture was evaporated and then extracted with ethyl acetate.
17. The organic phase was washed with 0.1 mol/L hydrochloric acid solution, saturated sodium bicarbonate solution and brine, and then dried with Na2SO4, and the solvent was removed in vacuo to yield the white solid (0.37 g, 77%).​

 

[onionexpress]

Labai ačiū ! Ar galite pateikti 1 kg galutinio produkto proporcijas ?

 

[MuricanSpirit]

Tiesiog viską padauginkite iš 370x (1000g/0,37g = 370 santykis) kaip "pagrindinę taisyklę".

Žinoma, esu tikras, kad kai kurie tirpikliai leidžia didesnio tankio mišinį, pvz. jums nereikės 370x daugiau etilacetato, bet greitai pastebėsite, kai tirpalas bus per daug prisotintas, bet turėkite omenyje, kad daugiau šilumos leidžia labiau prisotinti (nežinia kodėl).

 

[onionexpress]

Ačiū už tai, kad vertinu. Bet im naujokas ir man reikia konkrečios informacijos, kad išvengčiau klaidų.

 

[onionexpress]

Ar kas nors gali įkelti mokomąjį vaizdo įrašą? Esu naujokas ir nenoriu žinoti kiekvieno žingsnio (įskaitant reikalingą įrangą). Būčiau dėkingas ačiū daug

 

[William D.]

in PM

 

[00000000]

can u send me to pls ačiū.

 

[BackstagePanther]

Laba diena, ar tai yra analogas 5F-KUMIL-PEGAKLONUI (5F-SGT-151) ?
Ar ketinate įkelti ir jo sintezę? Būtų daugiau nei įdomu.
Ačiū už jūsų didžiulį darbą.

 

[G.Patton]

Jis turi skirtingą anglies skeletą

 

[BackstagePanther]

O, ką tik supratau, kad 5F-SGT-151 bazėje yra ir visas trečias benzeno žiedas. Įkeliu nomenklatūrą.
Galvojau, ar 5F-SGT-151 būtų galima pagaminti ir vietoj 1-bromo-5-fluoropentano naudoti kaip uodegą,
galėtume naudoti 1-bromo-6-fluoroheksaną. Ar tai suteiktų dar didesnį giminingumą receptoriams ir (arba) poveikį?

 

[G.Patton]

Remdamasis šiais duomenimis, sakyčiau, kad taip, bet tai tik hipotezė.

 

[Lordseeds]

 

[Lordseeds]

Taip, manau, kad to pakaks. Turiu dar vieną klausimą. Kurie kanabinoidai yra stipriausi?

 

[William D.]

adb-chminaca ir kai kurie klasikinio tipo noidai.

 

[king of synthesis]

Sveiki,
Ar šioje reakcijoje piridinas yra kalio tercbutoksido alternatyva?

 

[soebunies]

ne

 

[jejekororun]

I am interested in the synthesis of 5F-adb is there a simple reliable recipe?