Diisopropylethylamine → HCID 178461592, 화합물

HRID 522801노트

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HRID 522801 반응식
[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][NH:8]2)=[C:4](Cl)[N:3]=1.Cl.[CH3:13][C@@H:14]1[CH2:19][O:18][CH2:17][CH2:16][NH:15]1.C(N(C(C)C)CC)(C)C>C(O)(C)C.C(Cl)Cl>[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][NH:8]2)=[C:4]([N:15]2[CH2:16][CH2:17][O:18][CH2:19][C@H:14]2[CH3:13])[N:3]=1

참가 물질

6

반응물 3

HCID 81531DiisopropylethylamineHCID 57356922(3R)-3-Methylmorpholine hydrochlorideHCID 1784188752,6-dichloro-1H-purine

생성물 1

HCID 178461592HCID 178461592, 화합물수율 91%

시약·촉매·용매 2

HCID 3776Isopropanol용매HCID 6344Dichloromethane용매

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온도
75 °C

실험 절차

2,6-Dichloro-9H-purine (2.36 g, 12.5 mmol), (R)-3-methylmorpholin hydrochloride (1.89 g, 13.8 mmol), and diisopropylethylamine (5.46 mL, 31.3 mmol) were dissolved in 15 mL of isopropanol, and the reaction mixture was stirred for 18 hours at 75° C. The reaction mixture was then diluted with 200 mL of CH2Cl2. The organic solvents were washed with aqueous Na2CO3, followed by water and brine. Drying over Na2SO4, filtering and concentration under reduced pressure gave a residue, which was purified by column chromatography (150 g SiO2, CH2Cl2/EtOH/aq NH3 in a ratio of 96/4/0.1) to give the product as a solid (2.87 g, 91%).

후처리

  1. washThe organic solvents were washed with aqueous Na2CO3
  2. dry with materialDrying over Na2SO4
  3. filtrationfiltering
  4. concentrationconcentration under reduced pressure
  5. customgave a residue, which
  6. customwas purified by column chromatography (150 g SiO2, CH2Cl2/EtOH/aq NH3 in a ratio of 96/4/0.1)

출처 및 근거

ORD 기록
ord-96f55633c3ba4c54b37d56e267289d66
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09334271B2

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