Nicotinic acid, hydrazide → HCID 86757853、化合物

HRID 277112

反応式

HRID 277112 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+].[C:24]([NH:32][NH2:33])(=[O:31])[C:25]1[CH:30]=[CH:29][CH:28]=[N:27][CH:26]=1>C(Cl)(Cl)Cl.O1CCOCC1>[NH2:16][C:5](=[N:33][NH:32][C:24](=[O:31])[C:25]1[CH:30]=[CH:29][CH:28]=[N:27][CH:26]=1)[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

7

反応物 4

HCID 11112Nicotinic acid, hydrazideHCID 14798Sodium HydroxideHCID 516892Sodium BicarbonateHCID 700894412-(Phenylsulfonyl)-ethanimidic acid ethyl ester hydrochloride

生成物 1

HCID 86757853HCID 86757853、化合物収率 55%

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 312751,4-Dioxane溶媒

実験手順

A suspension of 23.6 g (0.089 mol) 2-(phenylsulfonyl)-ethanimidic acid ethyl ester hydrochloride in 300 ml chloroform was treated with 98 ml 1N aqueous sodium hydoxide. 200 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 13.5 g (0.098 mol) nicotinic acid hydrazide in 500 ml dioxane over night at 50° C. The resulting precipitate was filtered off and dried. A yield of 15.5 g (55%) nicotinic acid (1-amino-2-benzenesulfonyl-ethylidene)-hydrazide was obtained as white solid, MS m/e (%): 319 (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-da3a986cd3924997b9a302428823fde1
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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