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

HRID 1292336

反応式

HRID 1292336 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e7ca6f9b6cb74790b78a4231cd52599c
出典データセット
uspto-grants-1998_05
特許番号
US05756504

関連ノート

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