Hydrogen Peroxide → HCID 178429771、化合物
反応式
[CH3:1][C:2]1([CH:5]2[CH2:10][CH2:9][C:8](=[O:11])[CH2:7][CH2:6]2)[CH2:4][CH2:3]1.CCC(C)[BH-](C(C)CC)C(C)CC.[Li+].[OH-].[Na+].OO>C1COCC1.C(O)C.O>[CH3:1][C:2]1([C@@H:5]2[CH2:10][CH2:9][C@H:8]([OH:11])[CH2:7][CH2:6]2)[CH2:3][CH2:4]1参加物
8
実験手順
A solution of 4.0 g (26.3 mmol) of 4-(1-methylcyclopropyl)cyclohexanone in 30 ml of THF was added dropwise at -78° C. to 5.5 g (29.0 mmol) of L-Selectride (1M in THF) and the mixture was subsequently stirred for 3 hours. It was then heated to room temperature, and 4 ml of H2O, 15 ml of ethanol, 11 ml of 6N NaOH and 13 ml of 35% strength H2O2 solution were added in succession to the reaction solution. This solution was left to stand overnight and then subjected to aqueous workup. Extraction was carried out with methylene chloride, and the extract was dried and concentrated. 3.4 g (86% of theory) were obtained of a colorless crystal powder, m.p.: 56° to 57° C.
後処理
- waitThis solution was left
- waitto stand overnight
- extractionExtraction
- customthe extract was dried
- concentrationconcentrated
- custom3.4 g (86% of theory) were obtained of a colorless crystal powder, m.p.: 56° to 57° C.
出典と根拠
- ORDレコード
- ord-52ab13d1969b4553b3185ba39d940fd3
- 出典データセット
- uspto-grants-1999_03
- 特許番号
- US05889012
反応ノート
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