Trifluoroacetic acid → [4-fluoro-2-(tetrahydro-2H-pyran-4-yloxy)-phenyl]-(5,6,7,8-tetrahydro-pyrido[4',3':4,5]thieno[2,3-d]pyrimidin-4-yl)-amine

HRID 450574노트

반응식

HRID 450574 반응식
FC(F)(F)C(O)=O.C(OC([N:15]1[CH2:42][CH2:41][C:18]2[C:19]3[C:24]([NH:25][C:26]4[CH:31]=[CH:30][C:29]([F:32])=[CH:28][C:27]=4[O:33][CH:34]4[CH2:39][CH2:38][O:37][CH2:36][CH2:35]4)=[N:23][CH:22]=[N:21][C:20]=3[S:40][C:17]=2[CH2:16]1)=O)(C)(C)C>C(Cl)Cl>[F:32][C:29]1[CH:30]=[CH:31][C:26]([NH:25][C:24]2[C:19]3[C:18]4[CH2:41][CH2:42][NH:15][CH2:16][C:17]=4[S:40][C:20]=3[N:21]=[CH:22][N:23]=2)=[C:27]([O:33][CH:34]2[CH2:39][CH2:38][O:37][CH2:36][CH2:35]2)[CH:28]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 696691144-[4-Fluoro-2-(tetrahydro-2H-pyran-4-yloxy)-phenylamino]-5,8-dihydro-6H-pyrido[4',3':4,5]thieno[2,3-d]pyrimidine-7-carboxylic acid tert-butyl ester

생성물 1

HCID 46182217[4-fluoro-2-(tetrahydro-2H-pyran-4-yloxy)-phenyl]-(5,6,7,8-tetrahydro-pyrido[4',3':4,5]thieno[2,3-d]pyrimidin-4-yl)-amine수율 66.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

Trifluoroacetic acid (0.50 mL) was added into a solution of 4-[4-fluoro-2-(tetrahydro-2H-pyran-4-yloxy)-phenylamino]-5,8-dihydro-6H-pyrido[4′,3′:4,5]thieno[2,3-d]pyrimidine-7-carboxylic acid tert-butyl ester (0.031 g, 0.06 mmol) in DCM (1 mL) and the reaction mixture was stirred at ambient temperature for 2 hours. The reaction mixture was diluted with DCM and washed with 2M NaOH. The organic phase was dried (MgSO4), filtered and concentrated in vacuo. The residue was washed with hexane to afford the title compound as a white solid (0.016 g, 65%).

후처리

  1. washwashed with 2M NaOH
  2. dry with materialThe organic phase was dried (MgSO4)
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. washThe residue was washed with hexane

출처 및 근거

ORD 기록
ord-df3ac11150174c7dbffd833b59a82f48
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08486953B2

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