Triethylamine → Hex-5-yn-1-yl methanesulfonate

HRID 129264

反応式

HRID 129264 の反応式
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[CH2:6]([OH:12])[CH2:7][CH2:8][CH2:9][C:10]#[CH:11].C(N(CC)CC)C>ClCCl>[CH3:1][S:2]([O:12][CH2:6][CH2:7][CH2:8][CH2:9][C:10]#[CH:11])(=[O:4])=[O:3]

参加物

5

実験手順

A solution of methanesulphonyl chloride (23.7 ml) in dry dichloromethane (25 ml.) was added dropwise to a solution of hex-5-yn-1-ol (Lancaster Synthesis, 25 g) and triethylamine (47.3 ml) in dichloromethane (300 ml), stirred under a nitrogen atmosphere at -70°. The resulting mixture was allowed to warm to room temperature over 16 hours. The mixture was then washed with water, dilute hydrochloric acid, saturated sodium bicarbonate solution and brine before drying over anhydrous magnesium sulphate and evaporation in vacuo. Hex-5-ynyl methanesulphonate was obtained as an oil (43.6 g) and was used without purification.

後処理

  1. washThe mixture was then washed with water, dilute hydrochloric acid, saturated sodium bicarbonate solution and brine
  2. dry with materialbefore drying over anhydrous magnesium sulphate and evaporation in vacuo

出典と根拠

ORDレコード
ord-f34665ecde3e4391abcf6b27dc244d0d
出典データセット
uspto-grants-1995_11
特許番号
US05466710

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