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

HRID 129264

반응식

HRID 129264 반응식
[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]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 702345-Hexyn-1-ol

생성물 1

HCID 12714590Hex-5-yn-1-yl methanesulfonate

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f34665ecde3e4391abcf6b27dc244d0d
출처 데이터셋
uspto-grants-1995_11
특허 번호
US05466710

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