Diisopropylethylamine → HCID 178461592、化合物

HRID 522801ノート

反応式

HRID 522801 の反応式
[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

参加物

6

反応物 3

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

生成物 1

HCID 178461592HCID 178461592、化合物収率 91%

試薬・触媒・溶媒 2

HCID 3776Isopropanol溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
75 °C

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-96f55633c3ba4c54b37d56e267289d66
出典データセット
uspto-grants-2016_05
特許番号
US09334271B2

反応ノート

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