Toluene → HCID 13080730、化合物
反応式
C1(C)C=CC=CC=1.[CH3:8][Si:9]([CH3:32])([C:28]([CH3:31])([CH3:30])[CH3:29])[O:10][CH2:11][C@@H:12]1[C@@H:19]2[C@@H:15]([O:16][C:17](=[O:20])[CH2:18]2)[CH2:14][C@H:13]1[O:21][CH:22]1[CH2:27][CH2:26][CH2:25][CH2:24][O:23]1.[H-].C([Al+]CC(C)C)C(C)C.C1(C)C=CC=CC=1.S([O-])([O-])(=O)=O.[Na+].[Na+]>O.CO>[CH3:8][Si:9]([CH3:32])([C:28]([CH3:30])([CH3:29])[CH3:31])[O:10][CH2:11][C@@H:12]1[C@@H:19]2[C@@H:15]([O:16][CH:17]([OH:20])[CH2:18]2)[CH2:14][C@H:13]1[O:21][CH:22]1[CH2:27][CH2:26][CH2:25][CH2:24][O:23]1参加物
反応物 4
生成物 1
試薬・触媒・溶媒 2
反応条件
- 温度
- 0 °C
実験手順
An anhydrous toluene (315 mL) solution of the compound 1 (68.4 g) was cooled to around −60° C. in a dry ice-methanol bath, and then a diisobutyl aluminum hydride/toluene solution (0.99M, 209 mL) was added dropwise over 33 minutes. The mixture was stirred for 2 hours, and then to the reaction mixture was added dropwise methanol (3.2 mL) at −65° C. over 3 minutes to stop the reaction. The reaction liquid was raised to around 0° C., and water was then added dropwise in two parts (18.5 mL+18 mL) while the mixture was stirred. Thereto was added anhydrous sodium sulfate (7.4 g), and the mixture was stirred at room temperature for 1 hour, and filtered with Celite (trade name). The solid that was filtered off was washed with tetrahydrofuran (160 mL), and concentrated to obtain a titled compound (70.7 g) having the following physical property values.
後処理
- customthe reaction
- customThe reaction liquid
- stirringwas stirred
- stirringthe mixture was stirred at room temperature for 1 hour
- filtrationfiltered with Celite (trade name)
- filtrationThe solid that was filtered off
- washwas washed with tetrahydrofuran (160 mL)
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-522c256eaa23458292227c4446668319
- 出典データセット
- uspto-grants-2015_10
- 特許番号
- US09150537B2
反応ノート
読み込み中…