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

HRID 2248011ノート

反応式

HRID 2248011 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

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)

後処理

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

出典と根拠

ORDレコード
ord-e14be7d50ca149a4b74fff06f34dbd4f
出典データセット
uspto-grants-1991_08
特許番号
US05037845

反応ノート

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