Trifluoroacetic acid → (6-{4-[6-(4-Fluoro-phenyl)-2-(2-(R)-methyl-pyrrolidin-1-yl)-pyrimidin-4-yl]-3-(R)-methyl-piperazin-1-yl}-5-methyl-pyridin-3-yl)-acetic acid

HRID 2195063ノート

反応式

HRID 2195063 の反応式
C([O:5][C:6](=[O:41])[CH2:7][C:8]1[CH:9]=[N:10][C:11]([N:15]2[CH2:20][CH2:19][N:18]([C:21]3[CH:26]=[C:25]([C:27]4[CH:32]=[CH:31][C:30]([F:33])=[CH:29][CH:28]=4)[N:24]=[C:23]([N:34]4[CH2:38][CH2:37][CH2:36][C@H:35]4[CH3:39])[N:22]=3)[C@H:17]([CH3:40])[CH2:16]2)=[C:12]([CH3:14])[CH:13]=1)(C)(C)C.C(O)(C(F)(F)F)=O>C(Cl)Cl>[F:33][C:30]1[CH:29]=[CH:28][C:27]([C:25]2[N:24]=[C:23]([N:34]3[CH2:38][CH2:37][CH2:36][C@H:35]3[CH3:39])[N:22]=[C:21]([N:18]3[CH2:19][CH2:20][N:15]([C:11]4[N:10]=[CH:9][C:8]([CH2:7][C:6]([OH:41])=[O:5])=[CH:13][C:12]=4[CH3:14])[CH2:16][C@H:17]3[CH3:40])[CH:26]=2)=[CH:32][CH:31]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 59168306(6-{4-[6-(4-Fluoro-phenyl)-2-(2-(R)-methyl-pyrrolidin-1-yl)-pyrimidin-4-yl]-3-(R)-methyl-piperazin-1-yl)-5-methyl-pyridin-3-yl)-acetic acid tert-butyl ester

生成物 1

HCID 59168364(6-{4-[6-(4-Fluoro-phenyl)-2-(2-(R)-methyl-pyrrolidin-1-yl)-pyrimidin-4-yl]-3-(R)-methyl-piperazin-1-yl}-5-methyl-pyridin-3-yl)-acetic acid

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Stir a solution of (6-{4-[6-(4-fluoro-phenyl)-2-(2-(R)-methyl-pyrrolidin-1-yl)-pyrimidin-4-yl]-3-(R)-methyl-piperazin-1-yl}-5-methyl-pyridin-3-yl)-acetic acid tert-butyl ester (210 mg, 0.375 mmol) and 1 mL of TFA in DCM (10 mL) at room temperature for 16 h. Concentrate and partition between EtOAc and sat. NaHCO3. Dry the organic layer (Na2SO4) and concentrate under reduced pressure. Purify using flash chromatography eluting with MeOH-DCM (1:19) to give the title compound.

後処理

  1. concentrationConcentrate
  2. custompartition between EtOAc and sat. NaHCO3
  3. dry with materialDry the organic layer (Na2SO4)
  4. concentrationconcentrate under reduced pressure
  5. customPurify
  6. washeluting with MeOH-DCM (1:19)

出典と根拠

ORDレコード
ord-c22cb871cb0542119eaa1f92dbead623
出典データセット
uspto-grants-2012_12
特許番号
US08334382B2

反応ノート

読み込み中…