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Trifluoroacetic acid → HCID 178420614, 화합물

HRID 1809727
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HRID 1809727 반응식
[N:1]1([CH2:7][CH2:8][NH:9][C:10]2[N:15]=[C:14]3[N:16](COCC[Si](C)(C)C)[N:17]=[C:18]([C:19]4[CH:24]=[CH:23][CH:22]=[C:21]([NH:25][CH2:26][C:27]5[S:28][CH:29]=[CH:30][CH:31]=5)[CH:20]=4)[C:13]3=[CH:12][N:11]=2)[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.C(O)(C(F)(F)F)=O>ClCCl>[N:1]1([CH2:7][CH2:8][NH:9][C:10]2[N:15]=[C:14]3[NH:16][N:17]=[C:18]([C:19]4[CH:24]=[CH:23][CH:22]=[C:21]([NH:25][CH2:26][C:27]5[S:28][CH:29]=[CH:30][CH:31]=5)[CH:20]=4)[C:13]3=[CH:12][N:11]=2)[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1
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참가 물질

4

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HCID 6422Trifluoroacetic acidHCID 68108959(2-morpholin-4-yl-ethyl)-[3-{3-[(thiophen-2-ylmethyl)-amino]-phenyl}-1-(2-trimethylsilanyl-ethoxymethyl)-1H-pyrazolo[3,4-d]pyrimidin-6-yl]-amine

생성물 1

HCID 178420614HCID 178420614, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a stirred solution of (2-morpholin-4-yl-ethyl)-[3-{3-[(thiophen-2-ylmethyl)-amino]-phenyl}-1-(2-trimethylsilanyl-ethoxymethyl)-1H-pyrazolo[3,4-d]pyrimidin-6-yl]-amine (170 mg, 0.3 mmol) in dichloromethane (10 mL) was added TFA (10 mL) at room temperature. The resulting mixture was stirred for another three hours at this temperature. The solvent was evaporated under reduced pressure and the residue was dissolved in EtOAc (10 mL). The organic phase was washed with saturated aqueous NaHCO3 (3 mL), brine (5 mL) and dried over anhydrous Na2SO4, filtered and concentrated. It was purified by prep-HPLC to give (2-morpholin-4-yl-ethyl)-(3-{3-[(thiophen-2-ylmethyl)-amino]-phenyl}-1H-pyrazolo[3,4-d]pyrimidin-6-yl)-amine as yellow solid. (Yield 20 mg, 11.7%).

후처리

  1. customThe solvent was evaporated under reduced pressure
  2. dissolutionthe residue was dissolved in EtOAc (10 mL)
  3. washThe organic phase was washed with saturated aqueous NaHCO3 (3 mL), brine (5 mL)
  4. dry with materialdried over anhydrous Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customIt was purified by prep-HPLC

출처 및 근거

ORD 기록
ord-581abc5c7e6f46e7b750b23ef42413ea
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08362023B2

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