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Hydrochloric Acid → 4-chloro-6-(5-isopropyl-2-methylphenyl)-2-(3-methyl-1-tosyl-1H-indol-4-yl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine

HRID 80772
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HRID 80772 반응식
C(O)C.[CH:4]([C:7]1[CH:8]=[CH:9][C:10]([CH3:45])=[C:11]([N:13]2[CH2:44][CH2:43][C:16]3[N:17]=[C:18]([C:23]4[CH:31]=[CH:30][CH:29]=[C:28]5[C:24]=4[C:25]([CH3:42])=[CH:26][N:27]5[S:32]([C:35]4[CH:41]=[CH:40][C:38]([CH3:39])=[CH:37][CH:36]=4)(=[O:34])=[O:33])[N:19]=[C:20](OC)[C:15]=3[CH2:14]2)[CH:12]=1)([CH3:6])[CH3:5].Cl.[Cl-].[Cl:48]C=[N+](C)C>ClCCl.C(=O)(O)[O-].[Na+]>[Cl:48][C:20]1[C:15]2[CH2:14][N:13]([C:11]3[CH:12]=[C:7]([CH:4]([CH3:6])[CH3:5])[CH:8]=[CH:9][C:10]=3[CH3:45])[CH2:44][CH2:43][C:16]=2[N:17]=[C:18]([C:23]2[CH:31]=[CH:30][CH:29]=[C:28]3[C:24]=2[C:25]([CH3:42])=[CH:26][N:27]3[S:32]([C:35]2[CH:41]=[CH:40][C:38]([CH3:39])=[CH:37][CH:36]=2)(=[O:33])=[O:34])[N:19]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 77311Chloro-N,N-dimethylformiminium chlorideHCID 71240555HCID 71240555, 화합물

생성물 1

HCID 866902544-chloro-6-(5-isopropyl-2-methylphenyl)-2-(3-methyl-1-tosyl-1H-indol-4-yl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine

시약·촉매·용매 2

HCID 6344
Dichloromethane
용매
2회
HCID 516892Sodium Bicarbonate용매2회

반응 조건

온도
68 °C

실험 절차

Ethanol (4 mL) was added to 6-(5-isopropyl-2-methylphenyl)-4-methoxy-2-(3-methyl-1-tosyl-1H-indol-4-yl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine (0.92 g, 1.58 mmol) and then 12 N aqueous HCl (2 mL, 24 mmol) was added and the mixture was heated to 68° C. for ca. 15 hours. The reaction was then cooled to room temperature, diluted with dichloromethane, and neutralized via the slow addition of saturated aqueous sodium bicarbonate. The resulting layers were separated and the aqueous layer was extracted two additional times with dichloromethane. The organic layers were combined, dried over Na2SO4, filtered, and concentrated. The resulting residue was then dissolved in dichloromethane (20 mL) and cooled to 0° C. and N-chloromethylene-N,N-dimethyl ammonium chloride (Vilsmeier reagent) (0.41 g, 3.21 mmol) was added. The reaction was then placed at room temperature for 25 minutes. The reaction was then diluted with dichloromethane and saturated aqueous sodium bicarbonate. The resulting layers were separated and the aqueous layer was extracted one additional time with dichloromethane. The organic layers were combined, dried over Na2SO4 filtered and concentrated. The resulting residue was purified by silica gel flash chromatography (0-45% ethyl acetate/heptanes) to provide 4-chloro-6-(5-isopropyl-2-methylphenyl)-2-(3-methyl-1-tosyl-1H-indol-4-yl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine. MS (ESI+) m/z 585.2 (M+H)+.

후처리

  1. temperatureThe reaction was then cooled to room temperature
  2. customThe resulting layers were separated
  3. extractionthe aqueous layer was extracted two additional times with dichloromethane
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. dissolutionThe resulting residue was then dissolved in dichloromethane (20 mL)
  8. temperaturecooled to 0° C.
  9. customThe resulting layers were separated
  10. extractionthe aqueous layer was extracted one additional time with dichloromethane
  11. dry with materialdried over Na2SO4
  12. filtrationfiltered
  13. concentrationconcentrated
  14. customThe resulting residue was purified by silica gel flash chromatography (0-45% ethyl acetate/heptanes)

출처 및 근거

ORD 기록
ord-dea8ed04e1e14a8a8371e8ab0cbb3895
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08846656B2

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