Sodium Hydroxide → 2,4-Difluoro-benzoic acid (1-amino-2-benzenesulfonyl-ethylidene)-hydrazide

HRID 277100

反応式

HRID 277100 の反応式
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]=[C:33]([F:35])[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][C:33]([F:35])=[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]

参加物

6

反応物 4

HCID 14798Sodium HydroxideHCID 516892Sodium BicarbonateHCID 27369222,4-Difluorobenzoic acid hydrazideHCID 700894412-(Phenylsulfonyl)-ethanimidic acid ethyl ester hydrochloride

生成物 1

HCID 700885692,4-Difluoro-benzoic acid (1-amino-2-benzenesulfonyl-ethylidene)-hydrazide収率 42%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

A suspension of 15.3 g (0.058 mol) 2-(phenylsulfonyl)-ethanimidic acid ethyl ester hydrochloride in 125 ml chloroform was treated with 58.1 ml 1N aqueous sodium hydoxide. 18 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 10.0 g (0.058 mol) 2,4-difluorobenzoic acid hydrazide in 110 ml chloroform over night at 50° C. The resulting precipitate was filtered off and dried. A yield of 8.50 g (42%) 2,4-difluoro-benzoic acid (1-amino-2-benzenesulfonyl-ethylidene)-hydrazide was obtained as white solid. MS m/e (%): 354 (M+H+, 100).

後処理

  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

出典と根拠

ORDレコード
ord-2ea8e458666b4f0e9dd79ae524c2a16a
出典データセット
uspto-grants-2002_03
特許番号
US06355653B1

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