Neopentyl alcohol → 2,2-Dimethylpropyl trifluoromethanesulfonate

HRID 20411

반응식

HRID 20411 반응식
[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

반응물 3

HCID 6404Neopentyl alcoholHCID 79372,6-LutidineHCID 67749Trifluoromethanesulfonic anhydride

생성물 1

HCID 156962812,2-Dimethylpropyl trifluoromethanesulfonate수율 72%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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

  1. customAdd water to quench
  2. customthe reaction
  3. customseparate the organic layer
  4. extractionextract the aqueous layer with dichloromethane
  5. dry with materialdry (magnesium sulfate)
  6. filtrationfilter
  7. concentrationconcentrate
  8. custompurify
  9. 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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