Trifluoroacetic acid → HCID 178493513, 화합물

HRID 1778787노트

반응식

HRID 1778787 반응식
[F:1][C:2]1[C:7]([O:8][CH3:9])=[CH:6][C:5]([O:10][CH3:11])=[C:4]([F:12])[C:3]=1[C:13]1[N:18]=[C:17]2[NH:19][N:20]=[C:21]([C:22]3[CH:31]=[C:30]4[C:25]([CH2:26][CH2:27][N:28](C(OC(C)(C)C)=O)[CH2:29]4)=[CH:24][CH:23]=3)[C:16]2=[CH:15][N:14]=1.C(O)(C(F)(F)F)=O.[CH3:46][S:47](Cl)(=[O:49])=[O:48]>ClCCl.CO>[F:1][C:2]1[C:7]([O:8][CH3:9])=[CH:6][C:5]([O:10][CH3:11])=[C:4]([F:12])[C:3]=1[C:13]1[N:18]=[C:17]2[NH:19][N:20]=[C:21]([C:22]3[CH:31]=[C:30]4[C:25]([CH2:26][CH2:27][N:28]([S:47]([CH3:46])(=[O:49])=[O:48])[CH2:29]4)=[CH:24][CH:23]=3)[C:16]2=[CH:15][N:14]=1

참가 물질

6

반응물 3

HCID 6422Trifluoroacetic acidHCID 31297Methanesulfonyl chlorideHCID 178493512tert-butyl 7-[6-(2,6-difluoro-3,5-dimethoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidin-3-yl]-3,4-dihydroisoquinoline-2(1H)-carboxylate

생성물 1

HCID 178493513HCID 178493513, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

실험 절차

tert-Butyl 7-[6-(2,6-difluoro-3,5-dimethoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidin-3-yl]-3,4-dihydroisoquinoline-2(1H)-carboxylate (10.0 mg, 0.0191 mmol) in dichloromethane (0.10 mL) was treated with TFA (0.10 mL). The mixture was stirred at r.t. for 1 h. The volatiles were evaporated. The residue was dissolved in acetonitrile (0.5 mL) and N,N-diisopropylethylamine (30.0 μL). To the mixture was added methanesulfonyl chloride (2.0 μL, 0.026 mmol). The mixture was stirred at r.t. for 30 min, and then diluted with methanol, and purified by RP-HPLC (pH=10) to afford the desired product. LCMS (M+H)+=502.1.

후처리

  1. customThe volatiles were evaporated
  2. dissolutionThe residue was dissolved in acetonitrile (0.5 mL)
  3. stirringThe mixture was stirred at r.t. for 30 min
  4. custompurified by RP-HPLC (pH=10)

출처 및 근거

ORD 기록
ord-0d8ca70b511740faafef1e0e016157a0
출처 데이터셋
uspto-grants-2016_02
특허 번호
US09266892B2

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