Trifluoroacetic acid → HCID 178481638, 화합물

HRID 72691

반응식

HRID 72691 반응식
COC1C=CC(C[N:8]2[C:13]3[NH:14][N:15]=[C:16]([NH:17][C:18]4[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=4)[C:12]=3[C:11](=[O:24])[N:10]([CH3:25])[C:9]2=[O:26])=CC=1.C(O)(C(F)(F)F)=O.FC(F)(F)S(O)(=O)=O>C(Cl)Cl>[CH3:25][N:10]1[C:11](=[O:24])[C:12]2[C:16]([NH:17][C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)=[N:15][NH:14][C:13]=2[NH:8][C:9]1=[O:26]

참가 물질

5

반응물 3

HCID 6422Trifluoroacetic acidHCID 62406Trifluoromethanesulfonic acidHCID 178490875HCID 178490875, 화합물

생성물 1

HCID 178481638HCID 178481638, 화합물수율 96%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 7-(4-Methoxybenzyl)-5-methyl-3-(phenylamino)-1H-pyrazolo[3,4-d]pyrimidine-4,6(5H,7H)-dione (6.6 g, 17.5 mmol) in CH2Cl2 (200 mL) is added TFA (30 mL) slowly at room temperature, followed by adding trifluoromethanesulfonic acid (10 mL) dropwise. After the reaction-mixture is stirred at r.t. for 2 hours, solvent is removed under reduced pressure, and then 200 mL of 1N NaOH is added with cooling. The mixture is extracted with ethyl acetate five times, dried over Na2SO4, and then filtered. The filtrate is evaporated to dryness to give 4.3 g of crude product as white solids (Yield: 96%). MS (ESI) m/z 258.1 [M+H]+.

후처리

  1. customsolvent is removed under reduced pressure
  2. addition200 mL of 1N NaOH is added
  3. temperaturewith cooling
  4. extractionThe mixture is extracted with ethyl acetate five times
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. customThe filtrate is evaporated to dryness

출처 및 근거

ORD 기록
ord-a704007e81294b31bd1b4c2c7307d379
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08829008B2

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