Triethylamine → 2-(Prop-2-ynyloxy)ethyl methanesulfonate

HRID 1971688ノート

反応式

HRID 1971688 の反応式
[CH2:1]([O:4][CH2:5][CH2:6][OH:7])[C:2]#[CH:3].C(N(CC)CC)C.[CH3:15][S:16](Cl)(=[O:18])=[O:17]>C(OCC)C.O>[CH3:15][S:16]([O:7][CH2:6][CH2:5][O:4][CH2:1][C:2]#[CH:3])(=[O:18])=[O:17]

参加物

6

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 775962-Propynoxyethanol

生成物 1

HCID 866505712-(Prop-2-ynyloxy)ethyl methanesulfonate

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 3283Diethyl Ether溶媒

実験手順

A solution of 1.7 g of 11b and 3 ml of triethyl amine in 20 ml of diethyl ether was treated at 0° C. with 1.5 ml of methanesulfonyl chloride. The mixture was stirred for an additional 30 min and then diluted with 35 ml of water and extracted with ethyl acetate. The combined organic layers were washed with 1M aq. K2CO3 solution and water, dried and concentrated, to provide 2.45 of 11c as a colorless oil; Rf 0.45 (heptane/ethyl acetate 1/1).

後処理

  1. extractionextracted with ethyl acetate
  2. washThe combined organic layers were washed with 1M aq. K2CO3 solution and water
  3. customdried
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-1f68b330314f45c9b6cecca358262577
出典データセット
uspto-grants-2013_04
特許番号
US08431564B2

反応ノート

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