Hydrochloric Acid → HCID 44517481、化合物

HRID 877259ノート

反応式

HRID 877259 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[C:11](=[O:18])[N:10]([CH2:19][C:20]3[CH:25]=[CH:24][C:23]([CH:26]([CH:41]4[CH2:45][CH2:44][CH2:43][CH2:42]4)[C:27]([NH:29][CH2:30][C:31]4[CH:36]=[CH:35][C:34]([C:37]([O:39]C)=[O:38])=[CH:33][CH:32]=4)=[O:28])=[CH:22][CH:21]=3)[N:9]=2)=[CH:4][CH:3]=1.[OH-].[Na+].Cl>O1CCOCC1.O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[C:11](=[O:18])[N:10]([CH2:19][C:20]3[CH:25]=[CH:24][C:23]([CH:26]([CH:41]4[CH2:45][CH2:44][CH2:43][CH2:42]4)[C:27]([NH:29][CH2:30][C:31]4[CH:32]=[CH:33][C:34]([C:37]([OH:39])=[O:38])=[CH:35][CH:36]=4)=[O:28])=[CH:22][CH:21]=3)[N:9]=2)=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 58136535HCID 58136535、化合物

生成物 1

HCID 44517481HCID 44517481、化合物

試薬・触媒・溶媒 1

HCID 218864351,4-Dioxane--water (1/1)溶媒

実験手順

270 mg (0.435 mmol) of methyl 4-({[(4-{[4-(4-chlorophenyl)-1-oxophthalazin-2(1H)-yl]methyl}phenyl)(cyclopentyl)acetyl]amino}methyl)benzenecarboxylate (Example 112A) were dissolved in 10 ml of dioxane/water (3:1 v/v), and 0.652 ml (0.652 mmol) of 1 N aqueous sodium hydroxide solution was added. The mixture was stirred at room temperature overnight. The reaction mixture was then acidified with 1 N hydrochloric acid and extracted repeatedly with ethyl acetate. The combined organic phases were dried over sodium sulfate and concentrated under reduced pressure. This gave 269 mg of the target compound.

後処理

  1. extractionextracted repeatedly with ethyl acetate
  2. dry with materialThe combined organic phases were dried over sodium sulfate
  3. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-efa61b8e514346c9bf45c0b36a6fa014
出典データセット
uspto-grants-2015_03
特許番号
US08987256B2

反応ノート

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