Neopentyl alcohol → 2,2-Dimethylpropyl trifluoromethanesulfonate
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[F:1][C:2]([F:15])([F:14])[S:3]([O:6]S(C(F)(F)F)(=O)=O)(=[O:5])=[O:4].[CH2:16](O)[C:17]([CH3:20])([CH3:19])[CH3:18].N1C(C)=CC=CC=1C>ClCCl>[CH3:16][C:17]([CH3:20])([CH3:19])[CH2:18][O:6][S:3]([C:2]([F:15])([F:14])[F:1])(=[O:5])=[O:4]참가 물질
5
실험 절차
Add trifluoromethanesulphonic anhydride (1.12 mL, 6.8 mmol) to a solution of neopentylalcohol (0.5 g, 5.7 mmol) and 2,6-lutidine (0.7 mL, 6.8 mmol) in dichloromethane (10 mL) at −78° C. and stir for 1 hour. Add water to quench the reaction, separate the organic layer and extract the aqueous layer with dichloromethane. Combine the organic layers, dry (magnesium sulfate), filter, concentrate and purify (silica gel chromatography, eluting with 1:4 hexane:dichloromethane) to give the desired compound as an oil (0.9 g, 72% yield).
후처리
- customAdd water to quench
- customthe reaction
- customseparate the organic layer
- extractionextract the aqueous layer with dichloromethane
- dry with materialdry (magnesium sulfate)
- filtrationfilter
- concentrationconcentrate
- custompurify
- wash(silica gel chromatography, eluting with 1:4 hexane:dichloromethane)
출처 및 근거
- ORD 기록
- ord-6975154842644f7fbddb9e327f2bcaee
- 출처 데이터셋
- uspto-grants-2010_06
- 특허 번호
- US07745438B2
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