Potassium Carbonate → HCID 71599174、化合物

HRID 1428951ノート

反応式

HRID 1428951 の反応式
[CH2:1]([N:3]1[CH:7]=[C:6]([C:8]2[CH:13]=[CH:12][C:11]([F:14])=[C:10]([CH3:15])[CH:9]=2)[N:5]=[C:4]1[CH2:16][C:17]([OH:19])=O)[CH3:2].CCN(C(C)C)C(C)C.[N:29]1([C:35]2[N:40]=[CH:39][CH:38]=[CH:37][N:36]=2)[CH2:34][CH2:33][NH:32][CH2:31][CH2:30]1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C.ClCCl>[CH2:1]([N:3]1[CH:7]=[C:6]([C:8]2[CH:13]=[CH:12][C:11]([F:14])=[C:10]([CH3:15])[CH:9]=2)[N:5]=[C:4]1[CH2:16][C:17]([N:32]1[CH2:33][CH2:34][N:29]([C:35]2[N:36]=[CH:37][CH:38]=[CH:39][N:40]=2)[CH2:30][CH2:31]1)=[O:19])[CH3:2]

参加物

7

反応物 4

HCID 11430Potassium CarbonateHCID 81531DiisopropylethylamineHCID 887471-(2-Pyrimidinyl)piperazineHCID 86688152HCID 86688152、化合物

生成物 1

HCID 71599174HCID 71599174、化合物収率 70.6%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒

実験手順

50 mg (1-ethyl-4-(4-fluoro-3-methyl-phenyl)-1H-imidazol-2-yl)-acetic acid was dissolved in 2 mL DMF. 100 mg PFTU and 60 μL DIPEA were added to this solution and the mixture was stirred for 10 min at RT. 160 mg 2-piperazin-1-yl-pyrimidine was added and the reaction was stirred over night. Then, potassium carbonate solution (5%) and dichlormethane were added, the organic layer was separated and the solvent was removed. The residue was purified by HPLC and crystallized with diisopropylether to give 55 mg of the desired compound.

後処理

  1. stirringthe reaction was stirred over night
  2. customthe organic layer was separated
  3. customthe solvent was removed
  4. customThe residue was purified by HPLC
  5. customcrystallized with diisopropylether

出典と根拠

ORDレコード
ord-5ceb2e7350eb41cfb5dcb9d9a9e42b03
出典データセット
uspto-grants-2015_01
特許番号
US08937176B2

反応ノート

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