Triethylamine → Methanesulfonic acid 6-methyl-pyridin-3-ylmethyl ester
반응식
[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]=1참가 물질
5
실험 절차
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.
후처리
- filtrationThe slurry was then filtered
- customto remove triethylamine hydrochloride
- washthe cake washed four times with tetraydrofuran (21.6 kg)
- customAn aliquot was removed
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-8efbf6aca8164368b82e4dc1a0fd284a
- 출처 데이터셋
- uspto-grants-2012_01
- 특허 번호
- US08101750B2
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