Amlodipine → Amlodipine (S)-Tetrahydro-5-oxo-2-furancarboxylate

HRID 353986

反応式

HRID 353986 の反応式
[CH3:1][CH2:2][O:3][C:4]([C:6]1[CH:11]([C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:17]=2[Cl:18])[C:10]([C:19]([O:21][CH3:22])=[O:20])=[C:9]([CH3:23])[NH:8][C:7]=1[CH2:24][O:25][CH2:26][CH2:27][NH2:28])=[O:5].[O:29]=[C:30]1[O:34][C@H:33]([C:35]([OH:37])=[O:36])[CH2:32][CH2:31]1>C(OCC)(=O)C>[CH3:1][CH2:2][O:3][C:4]([C:6]1[CH:11]([C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:17]=2[Cl:18])[C:10]([C:19]([O:21][CH3:22])=[O:20])=[C:9]([CH3:23])[NH:8][C:7]=1[CH2:24][O:25][CH2:26][CH2:27][NH2:28])=[O:5].[O:29]=[C:30]1[O:34][C@H:33]([C:35]([O-:37])=[O:36])[CH2:32][CH2:31]1

参加物

4

反応物 2

HCID 2162AmlodipineHCID 636468(2S)-5-oxooxolane-2-carboxylic acid

生成物 1

HCID 86591093Amlodipine (S)-Tetrahydro-5-oxo-2-furancarboxylate収率 92.2%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

Amlodipine (10 g, 0.025 mole) was dissolved in ethyl acetate (100 ml) with stirring. The solution was adjusted to 3° C. and slowly added with (S)-tetrahydro-5-oxo-2-furancarboxylic acid (3.69 g, 0.028 mole) prepared according to Korean Pat. Publication No. 0159540 to obtain a clear solution. This reaction was stirred at 3° C. for 20 hour to produce precipitates. They were filtered off and washed with ethyl acetate (50 ml), followed by drying at 40° C. under vacuum to give 12.4 g of the title compound (Yield 92.0%).

後処理

  1. customwas adjusted to 3° C.
  2. customprepared
  3. custom0159540 to obtain a clear solution
  4. stirringThis reaction was stirred at 3° C. for 20 hour
  5. customto produce
  6. customprecipitates
  7. filtrationThey were filtered off
  8. washwashed with ethyl acetate (50 ml)
  9. customby drying at 40° C. under vacuum

出典と根拠

ORDレコード
ord-886e5c883b3442d4ba55543793030546
出典データセット
uspto-grants-2004_06
特許番号
US06756390B2

関連ノート

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