4-tert-Butylcyclohexanone → 4-Tert-butyl-1,1-difluorocyclohexane
反応式
[C:1]([CH:5]1CCC(=O)CC1)(C)([CH3:3])[CH3:2].C(N(S(F)(F)[F:18])CC)C.B(F)(F)F.CCOCC.[F:30][C:31]1[CH:36]=[CH:35][C:34](OC)=[CH:33][CH:32]=1>C(Cl)Cl>[F:30][C:31]1([F:18])[CH2:36][CH2:35][CH:34]([C:1]([CH3:5])([CH3:3])[CH3:2])[CH2:33][CH2:32]1参加物
6
実験手順
A solution of 4-t-butylcyclohexanone (308 mg, 2.0 mmol) in CH2Cl2 (10.0 mL) was added to diethylaminosulfur trifluoride (483 mg, 3.0 mmol ) at room temperature under N2. BF3.OEt2 (100 mL) was added and the mixture was stirred for 6 h at room temperature. The mixture was washed with saturated NaHCO3, dried (Na2SO4), filtered and evaporated in vacuo. Proton and Fluorine NMR with 4-fluoroanisole (2 mmol) as internal standard showed that a 67% yield of 1,1-difluoro-4-t-butylcyclohexane was obtained.
後処理
- washThe mixture was washed with saturated NaHCO3
- dry with materialdried (Na2SO4)
- filtrationfiltered
- customevaporated in vacuo
出典と根拠
- ORDレコード
- ord-e98883bcad9f48b1850604966c62e288
- 出典データセット
- uspto-grants-2001_04
- 特許番号
- US06222064B1
反応ノート
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