Sodium Hydroxide → thiophene-2-carboxylic acid N'-(2-benzenesulfonyl-1-imino-ethyl)-hydrazide

HRID 277028

반응식

HRID 277028 반응식
Cl.C(O[C:5](=[NH:16])[CH2:6][S:7]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)(=[O:9])=[O:8])C.[OH-].[Na+].C(=O)(O)[O-].[Na+].[S:24]1[CH:28]=[CH:27][CH:26]=[C:25]1[C:29]([NH:31][NH2:32])=[O:30]>C(Cl)(Cl)Cl>[C:10]1([S:7]([CH2:6][C:5]([NH:32][NH:31][C:29]([C:25]2[S:24][CH:28]=[CH:27][CH:26]=2)=[O:30])=[NH:16])(=[O:8])=[O:9])[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1

참가 물질

6

반응물 4

HCID 14798Sodium HydroxideHCID 73098Thiophene-2-carbohydrazideHCID 516892Sodium BicarbonateHCID 700894412-(Phenylsulfonyl)-ethanimidic acid ethyl ester hydrochloride

생성물 1

HCID 178511478thiophene-2-carboxylic acid N'-(2-benzenesulfonyl-1-imino-ethyl)-hydrazide

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

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).

후처리

  1. extractionthe mixture was extracted with chloroform
  2. dry with materialdried with sodium sulfate
  3. distillationthe solvents were distilled off under reduced pressure
  4. filtrationThe resulting precipitate was filtered off
  5. customdried

출처 및 근거

ORD 기록
ord-ce100ce763ad4cb998802e65655cf565
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06355653B1

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