Ethanol → 1,3-Benzodioxole-5-carboxylic acid, 6-methoxy-
反応式
[CH3:1][O:2][C:3]1[C:4]([C:12]([O:14]C)=[O:13])=[CH:5][C:6]2[O:10][CH2:9][O:8][C:7]=2[CH:11]=1.[OH-].[Na+].C(O)C>O>[CH3:1][O:2][C:3]1[C:4]([C:12]([OH:14])=[O:13])=[CH:5][C:6]2[O:10][CH2:9][O:8][C:7]=2[CH:11]=1参加物
5
実験手順
A mixture of methyl 6-methoxy-1,3-benzodioxole-5-carboxylate (3 g, 14 mmol), prepared as in Example 1, 20% sodium hydroxide (50 mL) and ethanol (25 mL) was heated 1 hour at reflux and then diluted with water, washed with diethyl ether (2×), treated with concentrated hydrochloric acid and cooled in an ice-bath. The solids were collected, washed with water (2×) and dried under vacuum at 70° C. to give 6-methoxy-1,3-benzodioxole-5-carboxylic acid (2.3 g, 12 mmol), m.p. 151° C.
後処理
- temperaturewas heated 1 hour
- temperatureat reflux
- washwashed with diethyl ether (2×)
- additiontreated with concentrated hydrochloric acid
- temperaturecooled in an ice-bath
- customThe solids were collected
- washwashed with water (2×)
- customdried under vacuum at 70° C.
出典と根拠
- ORDレコード
- ord-f94280474b7f4fe2a10aff68aa6ba646
- 出典データセット
- uspto-grants-1998_04
- 特許番号
- US05739336
反応ノート
読み込み中…