Tetrabutylammonium Fluoride → Methyl E4-[5-[2-(4-tert-butylbenzyloxy)phenyl]-3-(3,5-difluoro-4-hydroxybenzyl)pent-4-enyl]-benzoate
反応式
[C:1]([C:5]1[CH:53]=[CH:52][C:8]([CH2:9][O:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2/[CH:17]=[CH:18]/[CH:19]([CH2:32][C:33]2[CH:38]=[C:37]([F:39])[C:36]([O:40][Si](C(C)C)(C(C)C)C(C)C)=[C:35]([F:51])[CH:34]=2)[CH2:20][CH2:21][C:22]2[CH:31]=[CH:30][C:25]([C:26]([O:28][CH3:29])=[O:27])=[CH:24][CH:23]=2)=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].[F-].C([N+](CCCC)(CCCC)CCCC)CCC>C1COCC1>[C:1]([C:5]1[CH:6]=[CH:7][C:8]([CH2:9][O:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2/[CH:17]=[CH:18]/[CH:19]([CH2:32][C:33]2[CH:38]=[C:37]([F:39])[C:36]([OH:40])=[C:35]([F:51])[CH:34]=2)[CH2:20][CH2:21][C:22]2[CH:31]=[CH:30][C:25]([C:26]([O:28][CH3:29])=[O:27])=[CH:24][CH:23]=2)=[CH:52][CH:53]=1)([CH3:4])([CH3:2])[CH3:3]参加物
4
実験手順
780 mg (1.05 mmol) of methyl E-4-[5-[2-(4-tert-butylbenzyloxy)phenyl]-3-(3,5-difluoro-4-triisopropylsilanyloxybenzyl)pent-4-enyl]benzoate are introduced into 20 ml of THF at room temperature under argon, 2.11 ml (2.11 mmol) of a 1 M solution of tetra-n-butylammonium fluoride in THF are added, and the mixture is stirred at room temperature until reaction is complete. All the volatile components are then removed in vacuo. The resulting crude product is purified by preparative HPLC. 229 mg (37% of theory) of the title compound are obtained.
後処理
- customAll the volatile components are then removed in vacuo
- customThe resulting crude product is purified by preparative HPLC
出典と根拠
- ORDレコード
- ord-c67f009f71944fc298f713e35bb4652a
- 出典データセット
- uspto-grants-2012_05
- 特許番号
- US08173704B2
反応ノート
読み込み中…