Nicotinic acid, hydrazide → HCID 86757853, 화합물

HRID 277112

반응식

HRID 277112 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+].[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]

참가 물질

7

반응물 4

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

생성물 1

HCID 86757853HCID 86757853, 화합물수율 55%

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 312751,4-Dioxane용매

실험 절차

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).

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-da3a986cd3924997b9a302428823fde1
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06355653B1

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