Acetone → 6-(Hydroxymethyl)-2,3-dihydro-1H-inden-1-one
反応式
[C:1]1([CH3:11])[CH:6]=[CH:5][C:4](S(O)(=O)=O)=[CH:3][CH:2]=1.C(=O)([O-])[O-:13].[K+].[K+].[CH3:18][C:19]([CH3:21])=[O:20]>O>[OH:13][CH2:11][C:1]1[CH:2]=[C:21]2[C:4]([CH2:3][CH2:18][C:19]2=[O:20])=[CH:5][CH:6]=1参加物
5
実験手順
A solution of Example 28 (8.0 g, 38.7 mmol) and p-toluenesulfonic acid (7.4 g, 38.7 mmol) in a mixture of water (20 mL) and acetone (85 mL) was heated to reflux for about 1 hour. The mixture was concentrated under vacuum, diluted with water, and neutralized by careful addition of potassium carbonate (2.7 g, 19.4 mmol). The precipitate was collected by filtration, washed with minimal water and diethyl ether, and dried under vacuum to provide the desired product. MS (DCI-NH3): m/z 180 (M+NH4)+.
後処理
- temperaturewas heated
- temperatureto reflux for about 1 hour
- concentrationThe mixture was concentrated under vacuum
- additiondiluted with water
- filtrationThe precipitate was collected by filtration
- washwashed with minimal water and diethyl ether
- customdried under vacuum
出典と根拠
- ORDレコード
- ord-ddd5005a16b14830a0335f61a1857d1a
- 出典データセット
- uspto-grants-2008_12
- 特許番号
- US07468371B2
反応ノート
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