Potassium Hydroxide → 5-Fluoro-2-[2-(1-methylpiperidin-4-yloxy)-4-(pyrrolidin-1-yl)-benzoylamino]benzoic acid

HRID 644228ノート

反応式

HRID 644228 の反応式
[F:1][C:2]1[CH:3]=[CH:4][C:5]([NH:12][C:13](=[O:33])[C:14]2[CH:19]=[CH:18][C:17]([N:20]3[CH2:24][CH2:23][CH2:22][CH2:21]3)=[CH:16][C:15]=2[O:25][CH:26]2[CH2:31][CH2:30][N:29]([CH3:32])[CH2:28][CH2:27]2)=[C:6]([CH:11]=1)[C:7]([O:9]C)=[O:8].[OH-].[K+]>CCO.O>[F:1][C:2]1[CH:3]=[CH:4][C:5]([NH:12][C:13](=[O:33])[C:14]2[CH:19]=[CH:18][C:17]([N:20]3[CH2:24][CH2:23][CH2:22][CH2:21]3)=[CH:16][C:15]=2[O:25][CH:26]2[CH2:31][CH2:30][N:29]([CH3:32])[CH2:28][CH2:27]2)=[C:6]([CH:11]=1)[C:7]([OH:9])=[O:8]

参加物

5

反応物 2

HCID 14797Potassium HydroxideHCID 68534920Methyl 5-fluoro-2-[2-(1-methylpiperidin-4-yloxy)-4-(pyrrolidin-1-yl)benzoylamino]benzoate

生成物 1

HCID 685305135-Fluoro-2-[2-(1-methylpiperidin-4-yloxy)-4-(pyrrolidin-1-yl)-benzoylamino]benzoic acid

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

反応条件

温度
70 °C

実験手順

A solution of methyl 5-fluoro-2-[2-(1-methylpiperidin-4-yloxy)-4-(pyrrolidin-1-yl)benzoylamino]benzoate (7.8 g, 17 mmol) in EtOH (100 mL) and water (100 mL) was treated with KOH (4.8 g, 85 mmol) and stirred at 70° C. for 1 hour. The reaction was concentrated under vacuum, quenched with glacial acetic acid (5.1 g), and allowed to stand at ambient temperature for crystallization. The solid was filtered to recover 7.4 g (98%).

後処理

  1. concentrationThe reaction was concentrated under vacuum
  2. customquenched with glacial acetic acid (5.1 g)
  3. customto stand at ambient temperature for crystallization
  4. filtrationThe solid was filtered
  5. customto recover 7.4 g (98%)

出典と根拠

ORDレコード
ord-29111d7396b846a0b16758995c05629b
出典データセット
uspto-grants-2010_04
特許番号
US07700628B2

反応ノート

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