Potassium Carbonate → 2-(3-(4-Fluoro-3-methyl-phenyl)-5-phenyl-pyrazol-1-yl)-1-(4-(2-pyrimidinyl)-1-piperazinyl)-ethanon

HRID 68562

反応式

HRID 68562 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:12]=[C:11]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[N:10]([CH2:19][C:20](O)=[O:21])[N:9]=2)=[CH:4][C:3]=1[CH3:23].CCN(C(C)C)C(C)C.[N:33]1([C:39]2[N:44]=[CH:43][CH:42]=[CH:41][N:40]=2)[CH2:38][CH2:37][NH:36][CH2:35][CH2:34]1.C([O-])([O-])=O.[K+].[K+]>CN(C=O)C.C(Cl)Cl>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:12]=[C:11]([C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=3)[N:10]([CH2:19][C:20]([N:36]3[CH2:37][CH2:38][N:33]([C:39]4[N:40]=[CH:41][CH:42]=[CH:43][N:44]=4)[CH2:34][CH2:35]3)=[O:21])[N:9]=2)=[CH:4][C:3]=1[CH3:23]

参加物

7

反応物 4

HCID 11430Potassium CarbonateHCID 81531DiisopropylethylamineHCID 887471-(2-Pyrimidinyl)piperazineHCID 867626713-(4-Fluoro-3-methyl-phenyl)-5-phenyl-pyrazol-1-yl acetic acid

生成物 1

HCID 715717422-(3-(4-Fluoro-3-methyl-phenyl)-5-phenyl-pyrazol-1-yl)-1-(4-(2-pyrimidinyl)-1-piperazinyl)-ethanon

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒

実験手順

50 mg 3-(4-fluoro-3-methyl-phenyl)-5-phenyl-pyrazol-1-yl acetic acid was dissolved in 2 mL DMF. 83 mg PFTU and 33 μL DIPEA were added to this solution and the mixture was stirred for 15 min at RT. Then, 25 μL 2-(1-piperazinyl)-pyrimidine was added and stirring was continued for 8 h. Then, 1 mL of a K2CO3 solution (5%) and 10 mL CH2Cl2 were added, the organic phase was separated and washed two times with water. The solvent was removed and the residue was crystallized from ACN to yield 46 mg of the desired compound.

後処理

  1. stirringstirring
  2. waitwas continued for 8 h
  3. customthe organic phase was separated
  4. washwashed two times with water
  5. customThe solvent was removed
  6. customthe residue was crystallized from ACN

出典と根拠

ORDレコード
ord-8a49a257803b4b28833f6fe958b367d6
出典データセット
uspto-grants-2014_09
特許番号
US08822464B2

関連ノート

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