(Phenylsulfanyl)acetaldehyde → N-Methyl-4-[2-[2-(phenylthio)ethylidene]hydrazino]benzenemethanesulphonamide

HRID 2248011노트

반응식

HRID 2248011 반응식
[C:1]1([S:7][CH2:8][CH:9]=O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl.[NH:12]([C:14]1[CH:19]=[CH:18][C:17]([CH2:20][S:21]([NH:24][CH3:25])(=[O:23])=[O:22])=[CH:16][CH:15]=1)[NH2:13]>C(O)C.O>[CH3:25][NH:24][S:21]([CH2:20][C:17]1[CH:18]=[CH:19][C:14]([NH:12][N:13]=[CH:9][CH2:8][S:7][C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)=[CH:15][CH:16]=1)(=[O:23])=[O:22]

참가 물질

5

반응물 2

HCID 579732(Phenylsulfanyl)acetaldehydeHCID 142342634-Hydrazino-N-methylbenzenemethanesulfonamide hydrochloride

생성물 1

HCID 67923715N-Methyl-4-[2-[2-(phenylthio)ethylidene]hydrazino]benzenemethanesulphonamide수율 78.9%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

A solution of (phenylthio)acetaldehyde (6.05 g) in absolute ethanol (180 ml) was added over 10 min to a solution of 4-hydrazino-N-methylbenzenemethanesulphonamide hydrochloride (10 g) in water (180 ml) with cooling. After addition of the aldehyde was complete, the mixture was stirred at 5° for a period of 14 h. The precipitated solid was filtered off, washed with water (200 ml), hexane (200 ml) and dried in vacuo to give the title compound (10.95 g), m.p. 110°-112°. T.l.c. (B) Rf 0.5 (KMnO4)

후처리

  1. temperaturewith cooling
  2. filtrationThe precipitated solid was filtered off
  3. washwashed with water (200 ml), hexane (200 ml)
  4. customdried in vacuo

출처 및 근거

ORD 기록
ord-e14be7d50ca149a4b74fff06f34dbd4f
출처 데이터셋
uspto-grants-1991_08
특허 번호
US05037845

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