反応式
[Si:1]([O:8][CH2:9][C@H:10]([CH3:30])[O:11][C:12]1[CH:13]=[C:14]([CH:19]=[C:20]([O:22][CH2:23][C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[CH:21]=1)[C:15]([O:17]C)=[O:16])([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].O.O.[OH-].[Li+].C(O)(=O)CC(CC(O)=O)(C(O)=O)O>C1COCC1>[C:24]1([CH2:23][O:22][C:20]2[CH:19]=[C:14]([CH:13]=[C:12]([O:11][C@@H:10]([CH3:30])[CH2:9][O:8][Si:1]([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:2])[CH3:3])[CH:21]=2)[C:15]([OH:17])=[O:16])[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1参加物
6
反応物 4
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- 45 °C
実験手順
Methyl 3-((1S)-2-{[tert-butyl(dimethyl)silyl]oxy}-1-methylethoxy)-5-[(phenylmethyl)oxy]benzoate (3.0 g, 6.98 mmol) was dissolved in THF (50 mL) and water (10 mL) and lithium hydroxide monohydrate (586 mg, 13.95 mmol) added. The resultant mixture was heated with stirring at 45° C. for 2 hours, then at ambient temperature for 16 hours, and at 45° C. for a further 4 hours. Water (40 mL) was added and the solvent removed in vacuo. The resultant solution was acidified carefully with 1M citric acid (2 equivalents), washed with water and brine then dried (MgSO4), filtered and evaporated in vacuo to give the title compound as a colourless gum (2.58 g).
後処理
- waitat ambient temperature for 16 hours
- waitat 45° C. for a further 4 hours
- customthe solvent removed in vacuo
- washwashed with water and brine
- dry with materialthen dried (MgSO4)
- filtrationfiltered
- customevaporated in vacuo
出典と根拠
- ORDレコード
- ord-53255cda81cf4972872396b3a3987613
- 出典データセット
- uspto-grants-2011_05
- 特許番号
- US07943607B2
関連ノート
読み込み中…