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Water → 4-(2-Fluorophenyl)-7-(tetrahydro-2H-pyran-4-ylamino)-9H-pyrido[3,4-b]indole-1-carboxamide

HRID 2361264
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HRID 2361264 반응식
[NH2:1][C:2]1[CH:10]=[C:9]2[C:5]([C:6]3[C:14]([C:15]4[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=4[F:21])=[CH:13][N:12]=[C:11]([C:22]([NH2:24])=[O:23])[C:7]=3[NH:8]2)=[CH:4][CH:3]=1.[O:25]1[CH2:30][CH2:29][C:28](=O)[CH2:27][CH2:26]1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].O>O1CCCC1.ClCCl.C(OCC)(=O)C>[F:21][C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=1[C:14]1[C:6]2[C:5]3[C:9](=[CH:10][C:2]([NH:1][CH:28]4[CH2:29][CH2:30][O:25][CH2:26][CH2:27]4)=[CH:3][CH:4]=3)[NH:8][C:7]=2[C:11]([C:22]([NH2:24])=[O:23])=[N:12][CH:13]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 962WaterHCID 121599Tetrahydro-4H-pyran-4-one2회HCID 5049666Sodium triacetoxyborohydride2회HCID 679945367-amino-4-(2-fluorophenyl)-9H-pyrido[3,4-b]indole-1-carboxamide

생성물 1

HCID 706513764-(2-Fluorophenyl)-7-(tetrahydro-2H-pyran-4-ylamino)-9H-pyrido[3,4-b]indole-1-carboxamide수율 30.9%

시약·촉매·용매

3
HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 7-amino-4-(2-fluorophenyl)-9H-pyrido[3,4-b]indole-1-carboxamide (30.0 mg, 0.094 mmol), dihydro-2H-pyran-4(3H)-one (10.37 μL, 0.112 mmol), and sodium triacetoxyborohydride (39.7 mg, 0.187 mmol) in tetrahydrofuran (1 mL) and dichloromethane (1 mL) was stirred at rt for 16 hr. Additional dihydro-2H-pyran-4(3H)-one (10.37 μL, 0.112 mmol) and sodium triacetoxyborohydride (39.7 mg, 0.187 mmol) were added, and the mixture was stirred at room temperature for another 8 hr. To the reaction mixture was added water (2 mL), and the resulting mixture was stirred at room temperature for 20 min. It was diluted with ethyl acetate (50 mL), washed with saturated NaHCO3 solution (15 mL) and brine (15 mL), and dried over anhydrous MgSO4. Solvent was removed under vacuum, and the residue was subjected to prep. reverse phase HPLC purification. The correct fraction was concentrated under vacuum and basified with saturated NaHCO3 solution. The precipitating product (11.8 mg, 0.029 mmol, 30.8% yield) was collected as a yellow solid by suction filtration and dried at 50° C. under vacuum. LCMS (M+H)+=405.17. 1H NMR (500 MHz, DMSO-d6) δ: 11.30 (s, 1H), 8.23 (s, 1H), 8.11 (s, 1H), 7.70 (s, 1H), 7.65-7.61 (m, 2H), 7.49-7.42 (m, 2H), 6.98 (d, J=8.0 Hz, 1H), 6.94 (s, 1H), 6.46 (dd, J1=8.7 Hz, J2=1.5 Hz, 1H), 6.19 (br. s, 1H), 3.90 (m, 2H), 3.47 (m, 1H), 3.43 (m, 2H), 1.94 (m, 2H), 1.44 (m, 2H).

후처리

  1. stirringthe mixture was stirred at room temperature for another 8 hr
  2. stirringthe resulting mixture was stirred at room temperature for 20 min
  3. washwashed with saturated NaHCO3 solution (15 mL) and brine (15 mL)
  4. dry with materialdried over anhydrous MgSO4
  5. customSolvent was removed under vacuum
  6. customphase HPLC purification
  7. concentrationThe correct fraction was concentrated under vacuum

출처 및 근거

ORD 기록
ord-0425ae3ffe3c445fa951adf48e8b7b07
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08685969B2

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