Hydrochloric Acid → 4-[N'-(2-ethoxycarbonyl-1-acetyl ethylidene)hydrazino]benzene sulfonamide

HRID 399417

반응식

HRID 399417 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH2:11])(=[O:10])=[O:9])=[CH:4][CH:3]=1.Cl.[N:13]([O-])=O.[Na+].[CH2:17]([O:19][C:20](=[O:29])[CH2:21][CH:22](C(=O)C)[C:23](=[O:25])[CH3:24])[CH3:18]>C(O)C.O.C(O)C.N1C=CC=CC=1.O>[CH2:17]([O:19][C:20]([CH2:21][C:22](=[N:13][NH:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH2:11])(=[O:9])=[O:10])=[CH:4][CH:3]=1)[C:23](=[O:25])[CH3:24])=[O:29])[CH3:18]

참가 물질

9

반응물 4

HCID 313Hydrochloric AcidHCID 5333SulfanilamideHCID 87820Ethyl 3-acetyl-4-oxopentanoateHCID 23668193Sodium Nitrite

생성물 1

HCID 882324324-[N'-(2-ethoxycarbonyl-1-acetyl ethylidene)hydrazino]benzene sulfonamide

시약·촉매·용매 4

HCID 702Ethanol용매HCID 962Water용매HCID 1049Pyridine용매HCID 19096565Water ethanol용매

실험 절차

To a suspension of 10 g. (58.1 mmoles) of 4-aminobenzenesulfonamide in 50 ml of 1:1 ethanol/water was added 7.3 ml. of concentrated hydrochloric acid. To the cooled mixture was added in portions 4.41 g (63.9 mmoles) of sodium nitrite in 5 ml. of water. The mixture was allowed to come to room temperature and after 15 minutes was poured into a solution of 11.9 g. (63.9 mmoles) of ethyl-3-acetyl-4-oxopentanoate in 12.2 ml. of pyridine and 25 ml. of ethanol. An orange solid began to separate which was collected after 30 minutes by filtration. After drying, 24.3 g. of material was obtained.

후처리

  1. additionTo a suspension of 10 g
  2. additionwas poured into a solution of 11.9 g
  3. customto separate which
  4. filtrationwas collected after 30 minutes by filtration
  5. customAfter drying
  6. customof material was obtained

출처 및 근거

ORD 기록
ord-d87b2ffaa9194bad9f0689cf593347a0
출처 데이터셋
uspto-grants-1998_10
특허 번호
US05821243

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