Water → HCID 69879281、化合物
反応式
[BH4-].[Na+].[NH2:3][C:4]1[S:5][CH:6]=[C:7]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[C:8]=1[C:9]([O:11][CH2:12][CH3:13])=[O:10].O.C(=O)(O)[O-].[Na+].[CH:25]1([C:28](O)=O)[CH2:27][CH2:26]1>>[CH:25]1([CH2:28][NH:3][C:4]2[S:5][CH:6]=[C:7]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[C:8]=2[C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH2:27][CH2:26]1参加物
実験手順
Sodium borohydride (12.5 g) was added portionwise over 3 hours to a stirred solution of diethyl 2-aminothiophene-3,4-dicarboxyate (Example 36a, 25 g) in cyclopropane carboxylic acid (125 ml). The mixture was stirred at room temperature for 18 hours then further sodium borohydride (5 g) was added and stirring was continued at 50° C. for 16 hours. Further sodium borohydride (5 g) was again added and stirring was continued at 50° C. for 16 hours and then at room temperature for 3 days. Water (500 ml) was added, the mixture was neutralised with sodium bicarbonate and extracted with ether (2×250 ml). The organic extracts were dried over anhydrous magnesium sulfate, filtered and evaporated. The residue was purified by column chromatography over silica, eluting with ether/isohexane (2:3) to give the subtitle compound (12.10 g) as an oil.
後処理
- stirringstirring
- waitwas continued at 50° C. for 16 hours
- stirringstirring
- waitwas continued at 50° C. for 16 hours
- waitat room temperature for 3 days
- extractionextracted with ether (2×250 ml)
- dry with materialThe organic extracts were dried over anhydrous magnesium sulfate
- filtrationfiltered
- customevaporated
- customThe residue was purified by column chromatography over silica
- washeluting with ether/isohexane (2:3)
出典と根拠
- ORDレコード
- ord-f046d097ccf04b63b699c3aeaa0003ea
- 出典データセット
- uspto-grants-2001_10
- 特許番号
- US06300334B1
反応ノート
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