Methanesulfonyl chloride → HCID 20306015、化合物

HRID 1732338ノート

反応式

HRID 1732338 の反応式
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[CH3:6][O:7][C:8]1[CH:17]=[CH:16][CH:15]=[C:14]([O:18][CH3:19])[C:9]=1[O:10][CH2:11][CH2:12][OH:13]>N1C=CC=CC=1>[S:2]([O:13][CH2:12][CH2:11][O:10][C:9]1[C:8]([O:7][CH3:6])=[CH:17][CH:16]=[CH:15][C:14]=1[O:18][CH3:19])(=[O:4])(=[O:3])[CH3:1]

参加物

4

反応物 2

HCID 31297Methanesulfonyl chlorideHCID 142576012-(2,6-Dimethoxyphenoxy)ethan-1-ol

生成物 1

HCID 20306015HCID 20306015、化合物収率 40.5%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

Methanesulphonyl chloride (23 g.) was added dropwise to a stirred solution of 2-[2,6-dimethoxyphenoxy]ethanol (20 g.) (J. Med. Chem. 1969, 12, 326) in pyridine (50 ml.). The solution was left at room temperature for 60 hours, then the solvent evaporated under reduced pressure. The residue was taken up in chloroform, washed with water (3×100 ml.) and sodium bicarbonate solution (5%, 3×100 ml.), dried and the solvent evaporated. The residue was triturated with n-hexane and the solid collected to give 2-[2,6-dimethoxyphenoxy]-ethyl mesylate (11.3 g.) characterized spectroscopically.

後処理

  1. customthe solvent evaporated under reduced pressure
  2. washwashed with water (3×100 ml.) and sodium bicarbonate solution (5%, 3×100 ml.)
  3. customdried
  4. customthe solvent evaporated
  5. customThe residue was triturated with n-hexane
  6. customthe solid collected

出典と根拠

ORDレコード
ord-0376ac52247c46a4a070b6e6b4f1e4ab
出典データセット
uspto-grants-1980_12
特許番号
US04237138

反応ノート

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