Hydrochloric Acid → HCID 10488443、化合物
反応式
C[O:2][C:3]([C:5]1[CH:6]=[C:7]2[C:11](=[CH:12][C:13]=1[C:14]([O:16]C)=[O:15])[NH:10][CH:9]=[CH:8]2)=[O:4].C(O)C.[OH-].[Na+].Cl>O>[NH:10]1[C:11]2[C:7](=[CH:6][C:5]([C:3]([OH:4])=[O:2])=[C:13]([C:14]([OH:16])=[O:15])[CH:12]=2)[CH:8]=[CH:9]1参加物
6
実験手順
To a stirred solution of the dimethyl ester produced in step d (1.14 g, 4.9 mmol) in a 5:1 mixture of ethanol:water (12 ml) was added solid sodium hydroxide (0.49 g, 12.4 mmol). The solution was stirred at a gentle reflux for 3 h. The solution was acidified on cooling to pH2 with hydrochloric acid and then evaporated. The residue was azeotroped with ethanol and then toluene and dried under vacuum. The residue was then extracted with hot acetone (5×20 ml) and the combined extracts were evaporated to leave the title compound (870 mg).
後処理
- temperaturea gentle reflux for 3 h
- customevaporated
- customThe residue was azeotroped with ethanol
- dry with materialtoluene and dried under vacuum
- extractionThe residue was then extracted with hot acetone (5×20 ml)
- customthe combined extracts were evaporated
出典と根拠
- ORDレコード
- ord-70475fecee4b4994bf9d6367b034207a
- 出典データセット
- uspto-grants-1999_06
- 特許番号
- US05912260
反応ノート
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