1,2-Dichloroethane → 1-(2,4-Dimethoxyphenylacetyl)-4-(2-methylphenyl)piperazine-2-carboxamide

HRID 1292336

반응식

HRID 1292336 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]1[CH2:13][CH2:12][NH:11][CH:10]([C:14]([NH2:16])=[O:15])[CH2:9]1.[CH3:17][O:18][C:19]1[CH:24]=[C:23]([O:25][CH3:26])[CH:22]=[CH:21][C:20]=1[CH2:27][C:28](O)=[O:29].C(Cl)CCl.C(N(CC)CC)C>CN(C=O)C>[CH3:17][O:18][C:19]1[CH:24]=[C:23]([O:25][CH3:26])[CH:22]=[CH:21][C:20]=1[CH2:27][C:28]([N:11]1[CH2:12][CH2:13][N:8]([C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=2[CH3:1])[CH2:9][CH:10]1[C:14]([NH2:16])=[O:15])=[O:29]

참가 물질

6

반응물 4

HCID 111,2-DichloroethaneHCID 8471TriethylamineHCID 3505552-(2,4-Dimethoxyphenyl)acetic acidHCID 154305682-Carbamoyl-4-(2-methylphenyl)piperazine

생성물 1

HCID 189141491-(2,4-Dimethoxyphenylacetyl)-4-(2-methylphenyl)piperazine-2-carboxamide

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

4-(2-Methylphenyl)piperazine-2-carboxamide (39 mg, 0.18 mmol), 2,4-dimethoxyphenylacetic acid (42 mg, 0.21 mmol), EDC (42 mg, 0.22 mmol) and HBT (31 mg, 0.23 mmol) were combined in DMF (5 ml) and treated with triethylamine to adjust the pH to ca. 9 (moistened E. Merck colorpHast indicator). The mixture was stirred at ambient temperature for 64 hours. The solvent was removed in vacuo and the residue was chromatographed on silica gel eluted with 2% methanol in methylene chloride. The combined product fractions were evaporated to dryness in vacuo to provide the title compound.

후처리

  1. customThe solvent was removed in vacuo
  2. customthe residue was chromatographed on silica gel
  3. washeluted with 2% methanol in methylene chloride
  4. customThe combined product fractions were evaporated to dryness in vacuo

출처 및 근거

ORD 기록
ord-e7ca6f9b6cb74790b78a4231cd52599c
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05756504

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