Neopentyl alcohol → 2,2-Dimethylpropyl trifluoromethanesulfonate

HRID 20411

反応式

HRID 20411 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 156962812,2-Dimethylpropyl trifluoromethanesulfonate収率 72%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-6975154842644f7fbddb9e327f2bcaee
出典データセット
uspto-grants-2010_06
特許番号
US07745438B2

関連ノート

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