Sodium Hydroxide → 4-[2-[4-(4-Pyridyl)piperazin-1-yl]acetyl]phenoxyacetic acid

HRID 743807

반응식

HRID 743807 반응식
[N:1]1[CH:6]=[CH:5][C:4]([N:7]2[CH2:12][CH2:11][N:10]([CH2:13][C:14]([C:16]3[CH:27]=[CH:26][C:19]([O:20][CH2:21][C:22]([O:24]C)=[O:23])=[CH:18][CH:17]=3)=[O:15])[CH2:9][CH2:8]2)=[CH:3][CH:2]=1.[OH-].[Na+]>CO.O>[N:1]1[CH:6]=[CH:5][C:4]([N:7]2[CH2:8][CH2:9][N:10]([CH2:13][C:14]([C:16]3[CH:27]=[CH:26][C:19]([O:20][CH2:21][C:22]([OH:24])=[O:23])=[CH:18][CH:17]=3)=[O:15])[CH2:11][CH2:12]2)=[CH:3][CH:2]=1

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 22118604Methyl 4-[2-[4-(4-pyridyl)piperazin-1-yl]acetyl]phenoxyacetate

생성물 1

HCID 97987284-[2-[4-(4-Pyridyl)piperazin-1-yl]acetyl]phenoxyacetic acid

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

반응 조건

온도
4 °C

실험 절차

A stirred solution of the product of Example 1 (550 mg) in methanol (10 ml) was treated with a M sodium hydroxide solution (1.65 ml) and stirring continued for a further 2 hours. The mixture was diluted with water (10 ml) and the resulting solution concentrated in vacuo. Water (20ml) was added and then a M hydrochloric acid solution (1.65 ml). On cooling to 4° C., a solid precipitated. This mixture was concentrated in vacuo, the solid collected and washed with ice-water, then dried to give the title compound, 320 mg, as a solid: m.p. 294°-296° C.; NMR (d6DMSO+TFA) δ8.34(2H,d), 7.95(2H,d), 7.26(2H,d), 7.10(2H,d), 5.06(2H,s), 4.82(2H,s), 4.06(4H,bs), 3.52(4H,bs); m/e 356(M+H)+ ; calculated for C19H21N3O4 : C, 64.2; H, 6.0; N, 11.8. found: C, 64.1; H, 6.1; N, 11.6%.

후처리

  1. concentrationthe resulting solution concentrated in vacuo
  2. additionWater (20ml) was added
  3. customa solid precipitated
  4. concentrationThis mixture was concentrated in vacuo
  5. customthe solid collected
  6. washwashed with ice-water
  7. customdried

출처 및 근거

ORD 기록
ord-c19277b378ce467ebf64aee1fa4f0938
출처 데이터셋
uspto-grants-1996_09
특허 번호
US05556977

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