Triethylamine → Methanesulfonic acid 6-methyl-pyridin-3-ylmethyl ester
反応式
[CH3:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][OH:9])=[CH:4][CH:3]=1.C(N(CC)CC)C.[CH3:17][S:18](Cl)(=[O:20])=[O:19]>O1CCCC1>[CH3:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][O:9][S:18]([CH3:17])(=[O:20])=[O:19])=[CH:4][CH:3]=1参加物
5
実験手順
To a solution of (6-Methyl-pyridin-3-yl)-methanol (24.36 kg, 198 mol) dissolved in tetrahydrofuran (80 kg) under nitrogen at −3° C. was added triethylamine (22.14 kg, 218.8 mol) over 30 mins followed by methanesulphonyl chloride (23.16 kg, 202.2 mol) over 3 hr and the slurry stirred for an additional 30 mins. The slurry was then filtered to remove triethylamine hydrochloride and the cake washed four times with tetraydrofuran (21.6 kg). An aliquot was removed and concentrated and analysed.
後処理
- filtrationThe slurry was then filtered
- customto remove triethylamine hydrochloride
- washthe cake washed four times with tetraydrofuran (21.6 kg)
- customAn aliquot was removed
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-8efbf6aca8164368b82e4dc1a0fd284a
- 出典データセット
- uspto-grants-2012_01
- 特許番号
- US08101750B2
反応ノート
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