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HCID 66998054, 화합물 → HCID 24936717, 화합물

HRID 561033
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HRID 561033 반응식
C(O[C:6](=O)[N:7]([CH2:9][C:10]1[CH:11]=[N:12][C:13]([F:41])=[CH:14][C:15]=1[C:16]1[C:21]2[S:22][C:23]([C:25]3[C:30]([F:31])=[CH:29][N:28]=[C:27]([NH:32][CH2:33][CH2:34][N:35]4[CH2:39][CH2:38][NH:37][C:36]4=[O:40])[N:26]=3)=[CH:24][C:20]=2[CH:19]=[CH:18][CH:17]=1)C)(C)(C)C>C(Cl)Cl.C(O)(C(F)(F)F)=O>[F:31][C:30]1[C:25]([C:23]2[S:22][C:21]3[C:16]([C:15]4[C:10]([CH2:9][NH:7][CH3:6])=[CH:11][N:12]=[C:13]([F:41])[CH:14]=4)=[CH:17][CH:18]=[CH:19][C:20]=3[CH:24]=2)=[N:26][C:27]([NH:32][CH2:33][CH2:34][N:35]2[CH2:39][CH2:38][NH:37][C:36]2=[O:40])=[N:28][CH:29]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 66998054HCID 66998054, 화합물

생성물 1

HCID 24936717HCID 24936717, 화합물수율 78%

시약·촉매·용매 2

HCID 6344Dichloromethane용매2회HCID 6422Trifluoroacetic acid용매2회

실험 절차

Dissolve [4-(2-{5-fluoro-2-[2-(2-oxo-imidazolidin-1-yl)-ethylamino]-pyrimidin-4-yl}-benzo[b]thiophen-7-yl)-6-fluoro-pyridin-3-ylmethyl]-methyl-carbamic acid tert-butyl ester (0.19 g, 0.32 mmol) in dry CH2Cl2 (1.4 mL) and CF3COOH (1.4 mL). Stir at room temperature for 1 hour. Remove solvent completely. Dilute the trifluoro-acetic acid salt with CH2Cl2. Wash with saturated NaHCO3 solution, water and saturated aqueous sodium chloride. Dry with MgSO4. After filtration, remove solvent. Dry in vacuo overnight to afford the title compound (0.12 g, 78%). MS (ES) m/z 495 [M+1]+.

후처리

  1. washWash with saturated NaHCO3 solution, water and saturated aqueous sodium chloride
  2. dry with materialDry with MgSO4
  3. filtrationAfter filtration
  4. customremove solvent
  5. customDry in vacuo overnight

출처 및 근거

ORD 기록
ord-f7ce5f861f3e4912a0c09d38b95f06d7
출처 데이터셋
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08063212B2

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