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Acetyl chloride → HCID 59320892, 화합물

HRID 341187
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HRID 341187 반응식
[NH:1]1[CH2:6][CH2:5][CH:4]([O:7][C:8]2[CH:9]=[C:10]([C:14]3[CH:19]=[CH:18][N:17]4[C:20]([C:23]5[CH:24]=[C:25]([NH:29][C:30]([NH:32][CH2:33][C:34]([F:37])([F:36])[F:35])=[O:31])[CH:26]=[CH:27][CH:28]=5)=[CH:21][N:22]=[C:16]4[CH:15]=3)[CH:11]=[CH:12][CH:13]=2)[CH2:3][CH2:2]1.[C:38](Cl)(=[O:40])[CH3:39].CCN(CC)CC>CN(C=O)C>[C:38]([N:1]1[CH2:6][CH2:5][CH:4]([O:7][C:8]2[CH:9]=[C:10]([C:14]3[CH:19]=[CH:18][N:17]4[C:20]([C:23]5[CH:24]=[C:25]([NH:29][C:30]([NH:32][CH2:33][C:34]([F:35])([F:36])[F:37])=[O:31])[CH:26]=[CH:27][CH:28]=5)=[CH:21][N:22]=[C:16]4[CH:15]=3)[CH:11]=[CH:12][CH:13]=2)[CH2:3][CH2:2]1)(=[O:40])[CH3:39]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 59320856HCID 59320856, 화합물

생성물 1

HCID 59320892HCID 59320892, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 1-(3-{7-[3-(Piperidin-4-yloxy)-phenyl]-imidazo[1,2-a]pyridine-3-yl}-phenyl)-3-(2,2,2-trifluoro-ethyl)-urea (50 mg, 98 μmol in DMF(10 ml) was added acetyl chloride (6.3 μl, 82 μmol) and Et3N (14 μl). The reaction was stirred at room temperature for 3 h, then partitioned between EtOAc and H2O. The aqueous layer was again extracted with EtOAc, the organics combined, dried (MgSO4), filtered and the solvent removed in vacuo. The residue was purified by preparative HPLC to give the title compound (17.5 mg).

후처리

  1. custompartitioned between EtOAc and H2O
  2. extractionThe aqueous layer was again extracted with EtOAc
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. customthe solvent removed in vacuo
  6. customThe residue was purified by preparative HPLC

출처 및 근거

ORD 기록
ord-391921221e9c4e658096301cd7c029dc
출처 데이터셋
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08895745B2

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