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

HRID 220870노트

반응식

HRID 220870 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
60 °C

실험 절차

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%).

후처리

  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)

출처 및 근거

ORD 기록
ord-e429b9689f244d9da72c6cabadf57d2f
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08202858B2

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