Triethylamine → HCID 58248246、化合物
反応式
[O:1]1[CH2:5][CH2:4][C@@H:3]([OH:6])[CH2:2]1.C(N(CC)CC)C.[CH3:14][S:15](Cl)(=[O:17])=[O:16]>ClCCl>[CH3:14][S:15]([O:6][C@@H:3]1[CH2:4][CH2:5][O:1][CH2:2]1)(=[O:17])=[O:16]参加物
5
実験手順
(R)-Tetrahydrofuran-3-ol 1a (300 mg, 3.40 mmol) and triethylamine (687 mg, 6.80 mmol) were dissolved in 20 mL of dichloromethane in an ice bath, followed by addition of methanesulfonyl chloride (468 mg, 4.10 mmol). The reaction solution was warmed up to room temperature and stirred for 2 hours. The reaction solution was mixed with 10 mL of dichloromethane, washed with water (30 mL×3), dried with anhydrous magnesium sulphate, and filtered. The filtrate was concentrated under reduced pressure to obtain the title compound (R)-tetrahydrofuran-3-yl methanesulfonate 1b (520 mg) as a yellow oil, which was directly used in the next step without further purification.
後処理
- washwashed with water (30 mL×3)
- dry with materialdried with anhydrous magnesium sulphate
- filtrationfiltered
- concentrationThe filtrate was concentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-4586a53b8a354e42b08b54f65c7fdc4e
- 出典データセット
- uspto-grants-2015_09
- 特許番号
- US09139548B2
反応ノート
読み込み中…