Sodium Hydroxide → 1-cyclopropylmethyl-7-[4-(2-propoxyethoxy)phenyl]-2,3-dihydro-1H-1-benzazepine-4-carboxylic acid

HRID 586933ノート

反応式

HRID 586933 の反応式
[CH:1]1([CH2:4][N:5]2[C:11]3[CH:12]=[CH:13][C:14]([C:16]4[CH:21]=[CH:20][C:19]([O:22][CH2:23][CH2:24][O:25][CH2:26][CH2:27][CH3:28])=[CH:18][CH:17]=4)=[CH:15][C:10]=3[CH:9]=[C:8]([C:29]([O:31]C)=[O:30])[CH2:7][CH2:6]2)[CH2:3][CH2:2]1.[OH-].[Na+]>CO.C1COCC1>[CH:1]1([CH2:4][N:5]2[C:11]3[CH:12]=[CH:13][C:14]([C:16]4[CH:17]=[CH:18][C:19]([O:22][CH2:23][CH2:24][O:25][CH2:26][CH2:27][CH3:28])=[CH:20][CH:21]=4)=[CH:15][C:10]=3[CH:9]=[C:8]([C:29]([OH:31])=[O:30])[CH2:7][CH2:6]2)[CH2:3][CH2:2]1

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 22329229HCID 22329229、化合物

生成物 1

HCID 223290701-cyclopropylmethyl-7-[4-(2-propoxyethoxy)phenyl]-2,3-dihydro-1H-1-benzazepine-4-carboxylic acid収率 91.2%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

In methanol (25 ml) and THF (25 ml) was dissolved methyl 1-cyclopropylmethyl-7-[4-(2-propoxyethoxy)phenyl]-2,3-dihydro-1H-1-benzazepine-4-carboxylate (0.34 g). To the solution was added 1N sodium hydroxide solution (7.5 ml), and the mixture was stirred at room temperature overnight, heated at 50° C. for 1 hour, concentrated, which was neutralized with 1N hydrochloric acid and extracted with ethyl acetate. The organic layer was washed with water and saturated brine and dried with anhydrous magnesium sulfate. The solvent was evaporated to give 1-cyclopropylmethyl-7-[4-(2-propoxyethoxy)phenyl]-2,3-dihydro-1H-1-benzazepine-4-carboxylic acid (0.30 g) as yellow crystals.

後処理

  1. temperatureheated at 50° C. for 1 hour
  2. concentrationconcentrated
  3. extractionextracted with ethyl acetate
  4. washThe organic layer was washed with water and saturated brine
  5. dry with materialdried with anhydrous magnesium sulfate
  6. customThe solvent was evaporated

出典と根拠

ORDレコード
ord-4e41165d6462419aa8dbb38ae6778b60
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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