Methanesulfonyl chloride → 2-Methanesulfonyloxyethyl 2,2,2-trifluorethyl ether

HRID 2230664ノート

反応式

HRID 2230664 の反応式
[F:1][C:2]([F:9])([F:8])[CH2:3][O:4][CH2:5][CH2:6][OH:7].C(N(CC)C(C)C)(C)C.[CH3:19][S:20](Cl)(=[O:22])=[O:21]>ClCCl>[F:1][C:2]([F:9])([F:8])[CH2:3][O:4][CH2:5][CH2:6][O:7][S:20]([CH3:19])(=[O:22])=[O:21]

参加物

5

反応物 3

HCID 31297Methanesulfonyl chlorideHCID 81531DiisopropylethylamineHCID 2558542-(2,2,2-Trifluoroethoxy)ethan-1-ol

生成物 1

HCID 186737182-Methanesulfonyloxyethyl 2,2,2-trifluorethyl ether

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Combine 2-hydroxyethyl 2,2,2-trifluoroethyl ether (0.5 mmol) and N,N-diisopropylethylamine (1 mmol) in dichloromethane (20 mL). Cool in a ice-bath. Add dropwise, methanesulfonyl chloride (0.6 mmol). After 2 hours, extract with 1 M hydrochloric acid solution and 5% sodium bicarbonate solution. Dry the organic layer over MgSO4, filter, and concentrate in vacuo to give 2-methanesulfonyloxyethyl 2,2,2-trifluoroethyl ether.

後処理

  1. temperatureCool in a ice-bath
  2. additionAdd dropwise
  3. extractionextract with 1 M hydrochloric acid solution and 5% sodium bicarbonate solution
  4. dry with materialDry the organic layer over MgSO4
  5. filtrationfilter
  6. concentrationconcentrate in vacuo

出典と根拠

ORDレコード
ord-6e2f9263728a42919ccfb4c9bdd79901
出典データセット
uspto-grants-2002_07
特許番号
US06423704B1

反応ノート

読み込み中…