Trifluoroacetic acid → HCID 90402382, 화합물

HRID 2200581노트

반응식

HRID 2200581 반응식
[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

참가 물질

5

반응물 3

HCID 6422Trifluoroacetic acidHCID 62406Trifluoromethanesulfonic acidHCID 90403121HCID 90403121, 화합물

생성물 1

HCID 90402382HCID 90402382, 화합물수율 68.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-0c630f8237054eafabf6ca3911efc218
출처 데이터셋
uspto-grants-2016_06
특허 번호
US09359359B2

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