Potassium Carbonate → HCID 71599174, 화합물

HRID 1428951노트

반응식

HRID 1428951 반응식
[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]

참가 물질

7

반응물 4

HCID 11430Potassium CarbonateHCID 81531DiisopropylethylamineHCID 887471-(2-Pyrimidinyl)piperazineHCID 86688152HCID 86688152, 화합물

생성물 1

HCID 71599174HCID 71599174, 화합물수율 70.6%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5ceb2e7350eb41cfb5dcb9d9a9e42b03
출처 데이터셋
uspto-grants-2015_01
특허 번호
US08937176B2

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