Pyridine → N-isopropyl-N-(4-oxobutyl)-3,4-dichlorobenzenesulfonamide

HRID 2290954

反応式

HRID 2290954 の反応式
N1C=CC=CC=1.[CH:7]([N:10]([CH2:22][CH2:23][CH2:24][CH2:25][OH:26])[S:11]([C:14]1[CH:19]=[CH:18][C:17]([Cl:20])=[C:16]([Cl:21])[CH:15]=1)(=[O:13])=[O:12])([CH3:9])[CH3:8]>C(Cl)Cl.[O-2].[O-2].[O-2].[Cr+6]>[CH:7]([N:10]([CH2:22][CH2:23][CH2:24][CH:25]=[O:26])[S:11]([C:14]1[CH:19]=[CH:18][C:17]([Cl:20])=[C:16]([Cl:21])[CH:15]=1)(=[O:12])=[O:13])([CH3:9])[CH3:8]

参加物

5

反応物 2

HCID 1049PyridineHCID 13770966N-isopropyl-N-(4-hydroxybutyl)-3,4-dichlorobenzenesulfonamide

生成物 1

HCID 13770967N-isopropyl-N-(4-oxobutyl)-3,4-dichlorobenzenesulfonamide

試薬・触媒・溶媒 2

HCID 10219390chromium (VI) trioxide触媒HCID 6344Dichloromethane溶媒2 回

実験手順

Pyridine-chromic acid complex was prepared by adding chromium trioxide (26.4 g, 94 m. moles) to pyridine (41.76 g) in methylene chloride (660 ml). The reaction mixture was stirred at room temperature for 3/4 hours. Then N-isopropyl-N-(4-hydroxybutyl)-3,4-dichlorobenzenesulfonamide prepared in the preceding paragraph (15.01 g) in methylene chloride (150 ml) was added all at once. After 1/2 hour the liquid was decanted and washed with 5% aqueous NaOH, 5% aqueous HCl, 5% aqueous NaHCO3 and finally brine. After removal of solvent there was obtained N-isopropyl-N-(4-oxobutyl)-3,4-dichlorobenzenesulfonamide as a dark oil (9.01 g) which started to nicely crystallize but was used below without further purification.

後処理

  1. customPyridine-chromic acid complex was prepared
  2. additionwas added all at once
  3. customAfter 1/2 hour the liquid was decanted
  4. washwashed with 5% aqueous NaOH, 5% aqueous HCl, 5% aqueous NaHCO3 and finally brine
  5. customAfter removal of solvent there

出典と根拠

ORDレコード
ord-691aea981ce346a3b0539ec7acdd382e
出典データセット
uspto-grants-1986_10
特許番号
US04618711

関連ノート

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