Sodium Hydroxide → 4-[3-(4-Cyclopropyl-piperazin-1-yl)-propoxy]-3-fluoro-benzoic Acid

HRID 220870ノート

反応式

HRID 220870 の反応式
C([O:3][C:4](=[O:25])[C:5]1[CH:10]=[CH:9][C:8]([O:11][CH2:12][CH2:13][CH2:14][N:15]2[CH2:20][CH2:19][N:18]([CH:21]3[CH2:23][CH2:22]3)[CH2:17][CH2:16]2)=[C:7]([F:24])[CH:6]=1)C.[OH-].[Na+]>O1CCOCC1>[CH:21]1([N:18]2[CH2:17][CH2:16][N:15]([CH2:14][CH2:13][CH2:12][O:11][C:8]3[CH:9]=[CH:10][C:5]([C:4]([OH:25])=[O:3])=[CH:6][C:7]=3[F:24])[CH2:20][CH2:19]2)[CH2:23][CH2:22]1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 575554304-[3-(4-Cyclopropyl-piperazin-1-yl)-propoxy]-3-fluoro-benzoic Acid Ethyl Ester

生成物 1

HCID 575552724-[3-(4-Cyclopropyl-piperazin-1-yl)-propoxy]-3-fluoro-benzoic Acid収率 100%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
60 °C

実験手順

4-[3-(4-Cyclopropyl-piperazin-1-yl)-propoxy]-3-fluoro-benzoic acid ethyl ester from Example E48.2 (1.0 g, 2.9 mmol) was dissolved in dioxan (10 ml) and 2N NaOH solution (3 ml, 6.0 mmol) was added. The mixture was heated at 60° C. for 18 h then concentrated in vacuo. The residue was purified by flash chromatography on silica gel (eluant; 1% 35% ammonia:19% methanol:80% dichloro-methane) to yield the title compound (920 mg, 100%).

後処理

  1. concentrationthen concentrated in vacuo
  2. customThe residue was purified by flash chromatography on silica gel (eluant; 1% 35% ammonia:19% methanol:80% dichloro-methane)

出典と根拠

ORDレコード
ord-e429b9689f244d9da72c6cabadf57d2f
出典データセット
uspto-grants-2012_06
特許番号
US08202858B2

反応ノート

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