Sodium Hydroxide → 4-[3-[3-Hydroxy-4-(methoxycarbonyl)-2-propylphenoxy)propoxy]-alpha-oxobenzeneacetic acid
反応式
C([O:3][C:4](=[O:32])[C:5](=[O:31])[C:6]1[CH:11]=[CH:10][C:9]([O:12][CH2:13][CH2:14][CH2:15][O:16][C:17]2[CH:22]=[CH:21][C:20]([C:23]([O:25][CH3:26])=[O:24])=[C:19]([OH:27])[C:18]=2[CH2:28][CH2:29][CH3:30])=[CH:8][CH:7]=1)C.[OH-].[Na+]>CO>[OH:27][C:19]1[C:18]([CH2:28][CH2:29][CH3:30])=[C:17]([CH:22]=[CH:21][C:20]=1[C:23]([O:25][CH3:26])=[O:24])[O:16][CH2:15][CH2:14][CH2:13][O:12][C:9]1[CH:8]=[CH:7][C:6]([C:5](=[O:31])[C:4]([OH:32])=[O:3])=[CH:11][CH:10]=1参加物
4
実験手順
As in Example 19, a solution of 4-[3-[3-hydroxy-4-(methoxycarbonyl)-2-propylphenoxy)propoxy]-alpha-oxobenzeneacetic acid ethyl ester (0.3 g) in methanol (30 mL) was treated with 4N sodium hydroxide (0.53 mL) and then was stirred at room temperature for 1 hour. Most of the solvents were removed in vacuo, then the mixture was acidified with 3N hydrochloric acid and extracted with ethyl acetate. The dried (MgSO4) extracts were evaporated and the crude acid was crystallized from a carbon tetrachloride-hexane mixture containing a small amount of dichloromethane to yield 0.164 g of 4-[3-[3-hydroxy-4-(methoxycarbonyl)-2-propylphenoxy)propoxy]-alpha-oxobenzeneacetic acid, as a colorless solid, mp 86°-87° C.
後処理
- customMost of the solvents were removed in vacuo
- extractionextracted with ethyl acetate
- dry with materialThe dried (MgSO4) extracts
- customwere evaporated
- customthe crude acid was crystallized from a carbon tetrachloride-hexane mixture
- additioncontaining a small amount of dichloromethane
出典と根拠
- ORDレコード
- ord-4357bd1ae5c8411e8e06b12f04ebd48b
- 出典データセット
- uspto-grants-1994_09
- 特許番号
- US05344843
反応ノート
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