反応式
C([NH+](CC)CC)C.[C:8]12([CH2:18][O:19][C:20]([C:22]([F:28])([F:27])[S:23]([O-:26])(=[O:25])=[O:24])=[O:21])[CH2:17][CH:12]3[CH2:13][CH:14]([CH2:16][CH:10]([CH2:11]3)[CH2:9]1)[CH2:15]2.O.[Br-].[C:31]1([S+:37]([C:44]2[CH:49]=[CH:48][CH:47]=[CH:46][CH:45]=2)[C:38]2[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=2)[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1>C(Cl)(Cl)Cl>[C:8]12([CH2:18][O:19][C:20]([C:22]([F:28])([F:27])[S:23]([O-:26])(=[O:24])=[O:25])=[O:21])[CH2:17][CH:12]3[CH2:11][CH:10]([CH2:16][CH:14]([CH2:13]3)[CH2:15]1)[CH2:9]2.[C:44]1([S+:37]([C:31]2[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=2)[C:38]2[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=2)[CH:45]=[CH:46][CH:47]=[CH:48][CH:49]=1参加物
実験手順
Within a 1-L three-neck flask, 100 g (purity: 93%, 219 mmol, 1.0 eq) of the (adamantane-1-ylmethyl)oxycarbonyldifluoromethanesulfonic acid triethylammonium salt obtained in Example 1-c was dissolved in 300 g of chloroform. To the resulting solution, 250 g of water and 78.9 g (223 mmol, 1.05 eq) of triphenylsulfonium bromide were added. This reaction solution was stirred for 1 hour. After the reaction, the reaction solution was separated into an organic layer and an aqueous layer. The organic layer was washed with water, followed by distillating chloroform from the washed organic layer. The thus-obtained concentrated solution was dissolved in a mixed solvent of chloroform, ethyl acetate and diisopropyl ether and then recrystallized. With this, 119 g of target triphenylsulfonium (adamantane-1-ylmethyl)oxycarbonyldifluoromethanesulfonate was obtained (yield: 92%, purity: 99%).
後処理
- customAfter the reaction
- customthe reaction solution was separated into an organic layer
- washThe organic layer was washed with water
- dissolutionThe thus-obtained concentrated solution was dissolved in a mixed solvent of chloroform, ethyl acetate and diisopropyl ether
- customrecrystallized
出典と根拠
- ORDレコード
- ord-d6bb2c220ef44b70a03283ff2acd87a6
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08846966B2
関連ノート
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