Trifluoroacetic acid → HCID 90402382、化合物

HRID 2200581ノート

反応式

HRID 2200581 の反応式
[Cl:1][C:2]1[CH:42]=[CH:41][C:5]([CH2:6][N:7]2[C:15]3[C:14](=[O:16])[N:13](CC4C=CC(OC)=CC=4)[C:12](=[O:26])[N:11]([CH3:27])[C:10]=3[N:9]=[C:8]2[CH2:28][C:29]2[CH:34]=[C:33]([O:35][C:36]([F:39])([F:38])[F:37])[CH:32]=[CH:31][C:30]=2[F:40])=[CH:4][CH:3]=1.C(O)(C(F)(F)F)=O.FC(F)(F)S(O)(=O)=O>C(Cl)Cl>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:6][N:7]2[C:15]3[C:14](=[O:16])[NH:13][C:12](=[O:26])[N:11]([CH3:27])[C:10]=3[N:9]=[C:8]2[CH2:28][C:29]2[CH:34]=[C:33]([O:35][C:36]([F:38])([F:37])[F:39])[CH:32]=[CH:31][C:30]=2[F:40])=[CH:41][CH:42]=1

参加物

5

反応物 3

HCID 6422Trifluoroacetic acidHCID 62406Trifluoromethanesulfonic acidHCID 90403121HCID 90403121、化合物

生成物 1

HCID 90402382HCID 90402382、化合物収率 68.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 7-(4-chlorobenzyl)-8-(2-fluoro-5-(trifluoromethoxy)benzyl)-1-(4-methoxybenzyl)-3-methyl-1H-purine-2,6(3H,7H)-dione (71 mg, 0.118 mmol) in DCM (1 mL) was added TFA (0.3 mL) and trifluoromethanesulfonic acid (0.2 mL). The reaction was stirred at room temperature for 16 h. The mixture was concentrated and the residue was partitioned between DCM and aqueous sodium bicarbonate. The organic layer was dried and concentrated to give 7-(4-chlorobenzyl)-8-(2-fluoro-5-(trifluoromethoxy)benzyl)-3-methyl-1H-purine-2,6(3H,7H)-dione (39 mg, 68.4% yield) as a yellow syrup, which was directly without purification. LCMS retention time 1.686 min; LCMS MH+ 483.

後処理

  1. concentrationThe mixture was concentrated
  2. customthe residue was partitioned between DCM and aqueous sodium bicarbonate
  3. customThe organic layer was dried
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-0c630f8237054eafabf6ca3911efc218
出典データセット
uspto-grants-2016_06
特許番号
US09359359B2

反応ノート

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