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 450574ノート

反応式

HRID 450574 の反応式
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

参加物

4

反応物 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

生成物 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)-amine収率 66.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-df3ac11150174c7dbffd833b59a82f48
出典データセット
uspto-grants-2013_07
特許番号
US08486953B2

反応ノート

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