Sodium Hydroxide → HCID 22328990、化合物

HRID 587087ノート

反応式

HRID 587087 の反応式
[CH2:1]([O:3][CH2:4][CH2:5][CH2:6][N:7]1[C:13]2[CH:14]=[CH:15][C:16]([C:18]3[CH:23]=[CH:22][C:21]([O:24][CH2:25][CH2:26][O:27][CH2:28][CH2:29][CH3:30])=[CH:20][CH:19]=3)=[CH:17][C:12]=2[CH:11]=[C:10]([C:31]([O:33]C)=[O:32])[CH2:9][CH2:8]1)[CH3:2].[OH-].[Na+]>C1COCC1.CO>[CH2:1]([O:3][CH2:4][CH2:5][CH2:6][N:7]1[C:13]2[CH:14]=[CH:15][C:16]([C:18]3[CH:19]=[CH:20][C:21]([O:24][CH2:25][CH2:26][O:27][CH2:28][CH2:29][CH3:30])=[CH:22][CH:23]=3)=[CH:17][C:12]=2[CH:11]=[C:10]([C:31]([OH:33])=[O:32])[CH2:9][CH2:8]1)[CH3:2]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 22329178methyl 1-(3-ethoxypropyl)-7-[4-(2-propoxyethoxy)phenyl]-2,3-dihydro-1H-1-benzazepine-4-carboxylate

生成物 1

HCID 22328990HCID 22328990、化合物収率 84.6%

試薬・触媒・溶媒 1

HCID 21899815MeOH tetrahydrofuran溶媒

反応条件

温度
50 °C

実験手順

To a solution of methyl 1-(3-ethoxypropyl)-7-[4-(2-propoxyethoxy)phenyl]-2,3-dihydro-1H-1-benzazepine-4-carboxylate (475 mg) in a mixture of THF-methanol (5-10 ml) was added 1N sodium hydroxide solution (3.0 ml) at room temperature, and the mixture was stirred at 50° C. for 62 hours. After concentration under reduced pressure, to the mixture was added 1N hydrochloric acid (3.0 ml), and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine and dried with magnesium sulfate. After concentration under reduced pressure, the resulting crystals were collected by filtration. The crystals were washed with diisopropyl ether and hexane to give 1-(3-ethoxypropyl)-7-[4-(2-propoxyethoxy)phenyl]-2,3-dihydro-1H-1-benzazepine-4-carboxylic acid (390 mg) as yellow crystals.

後処理

  1. concentrationAfter concentration under reduced pressure
  2. additionto the mixture was added 1N hydrochloric acid (3.0 ml)
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with saturated brine
  5. dry with materialdried with magnesium sulfate
  6. concentrationAfter concentration under reduced pressure
  7. filtrationthe resulting crystals were collected by filtration
  8. washThe crystals were washed with diisopropyl ether and hexane

出典と根拠

ORDレコード
ord-4de7716c668b46c7ba13a136eb311e8c
出典データセット
uspto-grants-2005_08
特許番号
US06936602B1

反応ノート

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