Sodium Hydroxide → 5-Methyl-furan-2-carboxylic acid (1-amino-2-benzenesulfonyl-ethylidene)-hydrazide

HRID 277025

반응식

HRID 277025 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+].[CH3:24][C:25]1[O:29][C:28]([C:30]([NH:32][NH2:33])=[O:31])=[CH:27][CH:26]=1>C(Cl)(Cl)Cl>[NH2:16][C:5](=[N:33][NH:32][C:30]([C:28]1[O:29][C:25]([CH3:24])=[CH:26][CH:27]=1)=[O:31])[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 516892Sodium BicarbonateHCID 41592505-Methyl-2-furohydrazideHCID 700894412-(Phenylsulfonyl)-ethanimidic acid ethyl ester hydrochloride

생성물 1

HCID 867578445-Methyl-furan-2-carboxylic acid (1-amino-2-benzenesulfonyl-ethylidene)-hydrazide수율 82.8%

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

A suspension of 85.0 g (0.32 mol) 2-(phenylsulfonyl)-ethanimidic acid ethyl ester hydrochloride in 700 ml chloroform was treated with 320 ml 1N aqueous sodium hydroxide. 100 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. 17.8 g (0.078 Mol) of the resulting colorless oil was stirred together with 9.15 g (0.065 mol) 5-methyl-furan-2-carboxylic acid hydrazide in 115 ml chloroform for 24 hours at 50° C. The resulting precipitate was filtered off and dried. 17.3 g of 5-methyl-furan-2-carboxylic acid (1-amino-2-benzenesulfonyl-ethylidene)-hydrazide was obtained as white crystals. Mp.: 219-220° C.

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-7ecc062fc0854a2c86eb72796e15cb16
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06355653B1

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