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Potassium Hydroxide → HCID 71240555, 화합물

HRID 80774
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HRID 80774 반응식
Cl[C:2]1[C:3]2[CH2:31][N:30]([C:32]3[CH:37]=[C:36]([CH:38]([CH3:40])[CH3:39])[CH:35]=[CH:34][C:33]=3[CH3:41])[CH2:29][CH2:28][C:4]=2[N:5]=[C:6]([C:8]2[CH:16]=[CH:15][CH:14]=[C:13]3[C:9]=2[C:10]([CH3:27])=[CH:11][N:12]3[S:17]([C:20]2[CH:26]=[CH:25][C:23]([CH3:24])=[CH:22][CH:21]=2)(=[O:19])=[O:18])[N:7]=1.[CH3:42][O-:43].[Na+].[OH-].[K+].[OH-].[NH4+]>CO.CCOC(C)=O.O.ClCCl.[Cl-].[Na+].O>[CH:38]([C:36]1[CH:35]=[CH:34][C:33]([CH3:41])=[C:32]([N:30]2[CH2:29][CH2:28][C:4]3[N:5]=[C:6]([C:8]4[CH:16]=[CH:15][CH:14]=[C:13]5[C:9]=4[C:10]([CH3:27])=[CH:11][N:12]5[S:17]([C:20]4[CH:26]=[CH:25][C:23]([CH3:24])=[CH:22][CH:21]=4)(=[O:18])=[O:19])[N:7]=[C:2]([O:43][CH3:42])[C:3]=3[CH2:31]2)[CH:37]=1)([CH3:40])[CH3:39]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 4

HCID 14797Potassium HydroxideHCID 14923Ammonium HydroxideHCID 10942334Sodium MethoxideHCID 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

생성물 1

HCID 71240555HCID 71240555, 화합물

시약·촉매·용매 5

HCID 887
Methanol
용매
2회
HCID 962Water용매2회
HCID 6344Dichloromethane용매
HCID 8857Ethyl Acetate용매
HCID 57417360Sodium chloride; water용매

실험 절차

To a solution of 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, prepared as described in Example 17 (110 mg, 0.188 mmol) in methanol (5 mL) was added 25% sodium methoxide in methanol (40.6 mg, 0.188 mmol). The reaction was stirred for ca. 40 minutes at room temperature at which time the mixture was diluted with EtOAc and water. The layers were separated, and the organic layer was washed with brine, dried over Na2SO4, filtered, and concentrated. The resulting residue was added to a microwave vial, and diluted with EtOH (2 mL) and charged with KOH (ca. 100 mg, 1.75 mmol) and 28% ammonium hydroxide in water (1 mL, 7.25 mmol). The vial was sealed and heated via microwave irradiation at 100° C. for 45 minutes. The reaction mixture was cooled to room temperature and diluted with dichloromethane and brine. The 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 purified by silica gel flash chromatography (0-100% ethyl acetate/heptanes) and then further purified by reverse phase HPLC (20-100% MeCN/0.1% NH4OH in water to afford 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.

후처리

  1. customThe layers were separated
  2. washthe organic layer was washed with brine
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. additionThe resulting residue was added to a microwave vial
  7. additiondiluted with EtOH (2 mL)
  8. customThe vial was sealed
  9. temperatureheated via microwave irradiation at 100° C. for 45 minutes
  10. temperatureThe reaction mixture was cooled to room temperature
  11. customThe layers were separated
  12. extractionthe aqueous layer was extracted two additional times with dichloromethane
  13. dry with materialdried over Na2SO4
  14. filtrationfiltered
  15. concentrationconcentrated
  16. customThe resulting residue was purified by silica gel flash chromatography (0-100% ethyl acetate/heptanes)
  17. customfurther purified by reverse phase HPLC (20-100% MeCN/0.1% NH4OH in water

출처 및 근거

ORD 기록
ord-0a516fe914244675bf442490cb4ddd12
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08846656B2

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