Sodium Hydroxide → 2-Fluoro-benzoic acid (1-amino-2-benzenesulfonyl-ethylidene)-hydrazide

HRID 277104

반응식

HRID 277104 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+].[F:24][C:25]1[CH:34]=[CH:33][CH:32]=[CH:31][C:26]=1[C:27]([NH:29][NH2:30])=[O:28]>C(Cl)(Cl)Cl>[NH2:16][C:5](=[N:30][NH:29][C:27](=[O:28])[C:26]1[CH:31]=[CH:32][CH:33]=[CH:34][C:25]=1[F:24])[CH2:6][S:7]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)(=[O:9])=[O:8]

참가 물질

6

반응물 4

HCID 14798Sodium HydroxideHCID 1362882-FluorobenzhydrazideHCID 516892Sodium BicarbonateHCID 700894412-(Phenylsulfonyl)-ethanimidic acid ethyl ester hydrochloride

생성물 1

HCID 867578502-Fluoro-benzoic acid (1-amino-2-benzenesulfonyl-ethylidene)-hydrazide수율 75.1%

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

A suspension of 15.2 g (0.058 mol) 2-(phenylsulfonyl)-ethanimidic acid ethyl ester hydrochloride in 160 ml chloroform was treated with 57.7 ml 1N aqueous sodium hydoxide. 80 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 9.98 g (0.063 mol) 2-fluorobenzoic acid hydrazide in 65 ml chloroform over io night at 50° C. The resulting precipitate was filtered off and dried. A yield of 14.6 g 2-fluoro-benzoic acid (1-amino-2-benzenesulfonyl-ethylidene)-hydrazide was obtained as white solid. MS m/e (%): 336 (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-c2aecb6b3fd241cba4479e4faec34802
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06355653B1

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