反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A suspension of 13.2 g (0.05 mol) 2-(phenylsulfonyl)-ethanimidic acid ethyl ester hydrochloride in 110 ml chloroform was treated with 50 ml 1N aqueous sodium hydoxide. 20 ml of a saturated aqueous sodiumbicarbonate solution was added and the mixture was extracted with chloroform. The extracts were combined and dried with sodium sulfate and the solvents were distilled off under reduced pressure. The resulting colorless oil was stirred together with 7.82 g (0.05 mol) 2-thiophencarboxylic acid hydrazide in 75 ml chloroform for 24 hours at 50° C. The resulting precipitate was filtered off and dried. A quantitative yield thiophene-2-carboxylic acid N′-(2-benzenesulfonyl-1-imino-ethyl)-hydrazide was obtained as white crystals. MS m/e (%): 324 (M+H+, 100).
WORKUP
后处理
- extractionthe mixture was extracted with chloroform
- dry with materialdried with sodium sulfate
- distillationthe solvents were distilled off under reduced pressure
- filtrationThe resulting precipitate was filtered off
- customdried