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Methanesulfonyl chloride → 2-(3-Chloropropyl)-6-methylphenol

HRID 343485
ノート
印刷プレビュー

反応式

HRID 343485 の反応式
O[CH2:2][CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([CH3:11])[C:6]=1[OH:12].CS([Cl:17])(=O)=O>CO>[Cl:17][CH2:2][CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([CH3:11])[C:6]=1[OH:12]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 31297Methanesulfonyl chlorideHCID 543527972-(3-Hydroxypropyl)-6-methylphenol

生成物 1

HCID 544438172-(3-Chloropropyl)-6-methylphenol

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
110 °C

実験手順

A solution of N,N-dimethylaniline (24.0 mL) in toluene (20.0 mL) was bubbled with hydrochloride gas to prepare the corresponding hydrochloride. To the mixture were added 2-(3-hydroxypropyl)-6-methylphenol (20.0 g) and methanesulfonyl chloride (10.2 mL), and the resulting mixture was stirred at 110° C. for 1.5 hours. After cooling, methanol (2.4 mL) was added to the reaction mixture. The mixture was washed with distilled water, an aqueous sodium bicarbonate solution, distilled water and brine successively and then evaporated to give a solution of 2-(3-chloropropyl)-6-methylphenol (19.9 g) in toluene (21 g). NMR spectrum of this compound was identical with that of Reference Example 12.

後処理

  1. customA solution of N,N-dimethylaniline (24.0 mL) in toluene (20.0 mL) was bubbled with hydrochloride gas
  2. customto prepare the corresponding hydrochloride
  3. temperatureAfter cooling
  4. washThe mixture was washed with distilled water
  5. distillationan aqueous sodium bicarbonate solution, distilled water and brine successively
  6. customevaporated

出典と根拠

ORDレコード
ord-7179a961a0084adea8521b87d4c07711
出典データセット
uspto-grants-1999_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05861437

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート