Ammonium Chloride → 2-{4-[2-(3,5-Dimethyl-pyrazol-1-yl)-acetyl]-piperazin-1-yl}-benzoic acid methyl ester

HRID 2096261

반응식

HRID 2096261 반응식
[CH3:1][O:2][C:3](=[O:16])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[N:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1.[CH3:17][C:18]1[CH:22]=[C:21]([CH3:23])[N:20]([CH2:24][C:25](O)=[O:26])[N:19]=1.C(C1NC=CN=1)(C1NC=CN=1)=O.[NH4+].[Cl-]>CCOC(C)=O>[CH3:1][O:2][C:3](=[O:16])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[N:10]1[CH2:15][CH2:14][N:13]([C:25](=[O:26])[CH2:24][N:20]2[C:21]([CH3:23])=[CH:22][C:18]([CH3:17])=[N:19]2)[CH2:12][CH2:11]1

참가 물질

6

반응물 4

HCID 25517Ammonium ChlorideHCID 572875(3,5-Dimethyl-1H-pyrazol-1-yl)acetic acidHCID 5250894Bis-(1H-imidazol-2-YL)-methanoneHCID 10932975Methyl 2-(piperazin-1-yl)benzoate

생성물 1

HCID 665997292-{4-[2-(3,5-Dimethyl-pyrazol-1-yl)-acetyl]-piperazin-1-yl}-benzoic acid methyl ester수율 85.7%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

To a vial containing the 2-piperazin-1-yl-benzoic acid methyl ester (0.667 g, 3.03 mmol) is added a pre-mixed solution containing (3,5-dimethyl-pyrazol-1-yl)-acetic acid (0.428 g, 2.78 mmol) and carbonyl diimidazole (0.567 g, 3.50 mmol). The mixture is stirred overnight and then diluted with 200 mL of EtOAc followed by 200 mL of sat. NH4Cl. The organic phase is washed with 2×200 mL of H2O and 1×200 mL of brine. The organic phase is dried with MgSO4, filtered and concentrated to give 0.849 g of 2-{4-[2-(3,5-dimethyl-pyrazol-1-yl)-acetyl]-piperazin-1-yl}-benzoic acid methyl ester.

후처리

  1. additionis added a pre-mixed solution
  2. washThe organic phase is washed with 2×200 mL of H2O and 1×200 mL of brine
  3. dry with materialThe organic phase is dried with MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-e0d41b05ed414d209f28cc350e1aac4f
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08450317B2

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