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

HRID 277025

反応式

HRID 277025 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+].[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]

参加物

6

反応物 4

HCID 14798Sodium HydroxideHCID 516892Sodium BicarbonateHCID 41592505-Methyl-2-furohydrazideHCID 700894412-(Phenylsulfonyl)-ethanimidic acid ethyl ester hydrochloride

生成物 1

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

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

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.

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-7ecc062fc0854a2c86eb72796e15cb16
出典データセット
uspto-grants-2002_03
特許番号
US06355653B1

関連ノート

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