反応式
[OH-].[Na+].[OH:3][C:4]1([CH2:10][CH2:11][N:12]2[C:16](=[O:17])[CH2:15][S:14][CH:13]2[CH2:18][CH2:19][CH2:20][C:21]2[CH:31]=[CH:30][C:24]([C:25]([O:27]CC)=[O:26])=[CH:23][CH:22]=2)[CH2:9][CH2:8][CH2:7][CH2:6][CH2:5]1.CO.Cl>O>[OH:3][C:4]1([CH2:10][CH2:11][N:12]2[C:16](=[O:17])[CH2:15][S:14][CH:13]2[CH2:18][CH2:19][CH2:20][C:21]2[CH:22]=[CH:23][C:24]([C:25]([OH:27])=[O:26])=[CH:30][CH:31]=2)[CH2:5][CH2:6][CH2:7][CH2:8][CH2:9]1参加物
実験手順
Sodium hydroxide solution (5 N, 2.5 ml., 12.5 mmol.) is added to a stirred mixture of ethyl 4-{3-[3-[2-(1-hydroxycyclohexyl)ethyl]-4-oxo-2-thiazolidinyl]propyl}benzoate (2.48 g., 5.91 mmol.), methanol (25 ml.) and water (5 ml.). The resulting mixture is stirred at ambient temperature for 16 l hours. Then, it is diluted with water, acidified with diluted hydrochloric acid, and extracted with ether. The ethereal extract is washed with water, dried over anhydrous magnesium sulfate, and filtered. Upon cooling the filtrate, the title compound precipitates out as a white solid, which is collected by filtration (7.06 g., 2.57 mmol., 42%). The product is recrystallized from chloroform-ether, m.p. 147°-148° C., ir (KBr) 3320, 1700, 1650 cm-1, pmr (CDCl3) δ3.54 (2H, s), 4.70 (1H, m), 7.22 (2H, d), 8.00 (2H, d).
後処理
- extractionextracted with ether
- extractionThe ethereal extract
- washis washed with water
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltered
- temperatureUpon cooling the filtrate
- customthe title compound precipitates out as a white solid, which
- filtrationis collected by filtration (7.06 g., 2.57 mmol., 42%)
- customThe product is recrystallized from chloroform-ether, m.p. 147°-148° C., ir (KBr) 3320, 1700, 1650 cm-1, pmr (CDCl3) δ3.54 (2H, s), 4.70 (1H, m), 7.22 (2H, d), 8.00 (2H, d)
出典と根拠
- ORDレコード
- ord-11ca81f34b7c4d41aea0afe9d90a357a
- 出典データセット
- uspto-grants-1980_09
- 特許番号
- US04225609
関連ノート
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