Water → 4-(Bromomethyl)-1,1-difluorocyclohexane
反応式
C1(C)C=CC(S(O[CH2:11][CH:12]2[CH2:17][CH2:16][C:15]([F:19])([F:18])[CH2:14][CH2:13]2)(=O)=O)=CC=1.O.[Br-:22].[Li+].O>CC(C)=O>[Br:22][CH2:11][CH:12]1[CH2:17][CH2:16][C:15]([F:19])([F:18])[CH2:14][CH2:13]1参加物
5
実験手順
In 15 ml of acetone, 1.5 g of 4,4-difluorocyclohexylmethyl p-toluenesulfonate was dissolved. Thereto 1.6 g of lithium bromide monohydrate was added and the mixture was heated under reflux for 8 hours. After the reaction mixture was cooled to room temperature, water was added and the mixture was extracted with t-butyl methyl ether. The organic layer was washed with aqueous saturated sodium chloride, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 0.76 g of 4-bromomethyl-1,1-difluorocyclohexane.
後処理
- temperaturethe mixture was heated
- temperatureunder reflux for 8 hours
- extractionthe mixture was extracted with t-butyl methyl ether
- washThe organic layer was washed with aqueous saturated sodium chloride
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-2976c8297e0242aba5c661d1567f0e3a
- 出典データセット
- uspto-grants-2010_02
- 特許番号
- US07662402B2
反応ノート
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