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Trifluoroacetic acid → HCID 58405310, 화합물

HRID 44851
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HRID 44851 반응식
C(O)(C(F)(F)F)=O.[CH:8]1([N:13]2[C:22]3[N:21]=[C:20]([C:23]4[CH:28]=[CH:27][N:26]=[CH:25][C:24]=4[NH:29]C(=O)OC(C)(C)C)[N:19]=[CH:18][C:17]=3[N:16]([CH3:37])[C:15](=[O:38])[C@H:14]2[CH2:39][CH3:40])[CH2:12][CH2:11][CH2:10][CH2:9]1>C(Cl)Cl>[NH2:29][C:24]1[CH:25]=[N:26][CH:27]=[CH:28][C:23]=1[C:20]1[N:19]=[CH:18][C:17]2[N:16]([CH3:37])[C:15](=[O:38])[C@@H:14]([CH2:39][CH3:40])[N:13]([CH:8]3[CH2:12][CH2:11][CH2:10][CH2:9]3)[C:22]=2[N:21]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 58405528HCID 58405528, 화합물

생성물 1

HCID 58405310HCID 58405310, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Three mL of TFA was added to a solution of (R)-tert-butyl 4-(8-cyclopentyl-7-ethyl-5-methyl-6-oxo-5,6,7,8-tetrahydropteridin-2-yl)pyridin-3-ylcarbamate (Example 92, 760 mg) in 3 mL of DCM. The mixture was stirred for 4 h at rt, and the solvent was removed under reduced pressure. Aqueous Na2CO3 was added and extracted with EtOAc. The organic layer was dried with Na2SO4, concentrated and the residue was purified by silica column to give the title compound. LCMS (0.05% TFA): 353.0 m/z (M+H)+; 1H-NMR (CDCl3, 500 MHz): δ: 8.17 (s, 1H), 8.08 (d, 1H, J=5 Hz), 7.99 (d, 1H, J=5 Hz), 7.94 (s, 1H), 6.23 (s, 2H), 4.48 (m, 1H), 4.32 (m, 1H), 3.39 (s, 3H), 2.0-1.69 (m, 10H), 0.88 (t, 3H, J=7.5 Hz).

후처리

  1. customthe solvent was removed under reduced pressure
  2. additionAqueous Na2CO3 was added
  3. extractionextracted with EtOAc
  4. dry with materialThe organic layer was dried with Na2SO4
  5. concentrationconcentrated
  6. customthe residue was purified by silica column

출처 및 근거

ORD 기록
ord-8480fff61734432fb2841d2366cefbe0
출처 데이터셋
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08541418B2

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