Water → 2-chloro-N-(4-chlorobutyl-sulphonyl)-4-methyl-aniline

HRID 1629867

反応式

HRID 1629867 の反応式
[Cl:1][C:2]1[CH:8]=[C:7]([CH3:9])[CH:6]=[CH:5][C:3]=1[NH2:4].[Cl:10][CH2:11][CH2:12][CH2:13][CH2:14][S:15](Cl)(=[O:17])=[O:16].O>N1C=CC=CC=1>[Cl:1][C:2]1[CH:8]=[C:7]([CH3:9])[CH:6]=[CH:5][C:3]=1[NH:4][S:15]([CH2:14][CH2:13][CH2:12][CH2:11][Cl:10])(=[O:17])=[O:16]

参加物

5

反応物 3

HCID 962WaterHCID 120072-Chloro-p-toluidineHCID 742124-Chlorobutane-1-sulphonyl chloride

生成物 1

HCID 670486822-chloro-N-(4-chlorobutyl-sulphonyl)-4-methyl-aniline

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

1.30 ml (10.7 mmol) 2-chloro-4-methyl-aniline are placed in 30 ml of pyridine, combined with 2.67 g (10.5 mmol) 75% m 4-chlorobutyl-sulphonic acid chloride and stirred for 16 hours at ambient temperature. The reaction mixture is poured into water and extracted with ethyl acetate. The combined organic phases are washed with 6-molar hydrochloric acid, dried over sodium sulphate and evaporated down i. vac. The residue is purified by chromatography on silica gel (eluting gradient: petroleum ether/ethyl acetate=9:1->7:3).

後処理

  1. extractionextracted with ethyl acetate
  2. washThe combined organic phases are washed with 6-molar hydrochloric acid
  3. dry with materialdried over sodium sulphate
  4. customevaporated down i
  5. customThe residue is purified by chromatography on silica gel (eluting gradient: petroleum ether/ethyl acetate=9:1->7:3)

出典と根拠

ORDレコード
ord-fd801bc6111a4d088dd1f7c4f6030fce
出典データセット
uspto-grants-2014_07
特許番号
US08791103B2

関連ノート

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