HCID 11984299、化合物 → HCID 68955504、化合物

HRID 1453889ノート

反応式

HRID 1453889 の反応式
[CH2:1]([O:8][C:9]1[C:10]([C:27]([O:29]C)=O)=[N:11][NH:12][C:13]=1[C:14]([N:16]([CH2:18][CH:19](O)[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][N:21]=1)[CH3:17])=[O:15])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.[F:32][C:33]1[CH:40]=[CH:39][C:36]([CH2:37][NH2:38])=[C:35]([C:41]([NH:43][CH3:44])=[O:42])[CH:34]=1>>[CH2:1]([O:8][C:9]1[C:10]([C:27]([NH:38][CH2:37][C:36]2[CH:39]=[CH:40][C:33]([F:32])=[CH:34][C:35]=2[C:41]([NH:43][CH3:44])=[O:42])=[O:29])=[N:11][N:12]2[CH:19]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][N:21]=3)[CH2:18][N:16]([CH3:17])[C:14](=[O:15])[C:13]=12)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

3

反応物 2

HCID 11984299HCID 11984299、化合物HCID 178499184HCID 178499184、化合物

生成物 1

HCID 68955504HCID 68955504、化合物

実験手順

The title compound was prepared from methyl 4-(benzyloxy)-5-{[(2-hydroxy-2-pyridin-2-ylethyl)(methyl)amino]carbonyl}-1H-pyrazole-3-carboxylate using a procedure similar to that described in Example 43, Steps 2-4, except that 4-fluoro-2-[(methylamino)carbonyl]benzylamine hydrochloride was used in place of 4-fluorobenzylamine. Purification was achieved by removing the solvent in vacuo, and purifying the resulting residue by reverse phase chromatography on a C-18 column using a gradient elution of 95-5% H2O (0.1% TFA)/CH3CN (0.1% TFA). Collection and concentration of the appropriate fractions afforded the product. ES MS (M+1)=543.

後処理

  1. customPurification
  2. customby removing the solvent in vacuo
  3. custompurifying the resulting residue by reverse phase chromatography on a C-18 column
  4. washa gradient elution of 95-5% H2O (0.1% TFA)/CH3CN (0.1% TFA)
  5. customCollection and concentration of the appropriate fractions
  6. customafforded the product

出典と根拠

ORDレコード
ord-7e4211e79039485f8e397b954cbbfc61
出典データセット
uspto-grants-2009_01
特許番号
US07476666B2

反応ノート

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