تفاعل #66210

معادلة التفاعل

ethyl 1,2,3,6-tetrahydroazepino[4,5-b]indole-5-carboxylate

Lawesson's reagent

→

1,2,3,6-tetrahydroazepino[4,5-b]indole-5-carbothioic acid O-ethyl ester

المردود 5.0%

المذيبات

toluene

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe resulting suspension was heated
2. 2
   درجة الحرارةto reflux under nitrogen for 24 hours
3. 3
   أخرىSolvent was evaporated
4. 4
   أخرىto give the crude product, which
5. 5
   أخرىwas purified by column chromatography on silica gel eluting with MeOH-DCM (1:19)

الإجراء التجريبي

To a solution of ethyl 1,2,3,6-tetrahydroazepino[4,5-b]indole-5-carboxylate (0.51 g, 2 mmol) in toluene (20 mL) was added Lawesson's reagent (1.45 g, 3.6 mmol). The resulting suspension was heated to reflux under nitrogen for 24 hours. Solvent was evaporated to give the crude product, which was purified by column chromatography on silica gel eluting with MeOH-DCM (1:19) to give 1,2,3,6-tetrahydroazepino[4,5-b]indole-5-carbothioic acid O-ethyl ester (27 mg); MS (ES): 273 (MH+).

المصدر