Diisopropylethylamine → HCID 178461592、化合物

HRID 1945690ノート

反応式

HRID 1945690 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.[CH3:12][C@@H:13]1[CH2:18][O:17][CH2:16][CH2:15][NH:14]1.CCN(C(C)C)C(C)C>>[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][NH:8]2)=[C:4]([N:14]2[CH2:15][CH2:16][O:17][CH2:18][C@H:13]2[CH3:12])[N:3]=1

参加物

4

反応物 3

HCID 81531DiisopropylethylamineHCID 641498(R)-3-MethylmorpholineHCID 1784188752,6-dichloro-1H-purine

生成物 1

HCID 178461592HCID 178461592、化合物収率 31.2%

反応条件

温度
80 °C

実験手順

A mixture of 2,6-dichloro-9H-purine (2.18 g, 11.53 mmol), (R)-3-methylmorpholine (1.40 g, 13.84 mmol) and DIPEA (2.57 mL, 14.99 mmol) in IMS (50 mL) were heated at 80° C. for 8 h. The reaction mixture was concentrated in vacuo to a reduced volume and the residue partitioned between EtOAc and H2O. The organic phase was dried (Na2SO4) and concentrated in vacuo. The resulting residue was purified by column chromatography (Si—PCC, MeOH:EtOAc, 0-10%) affording the title compound as an off-white solid (914 mg, 31%). LCMS (method H): RT 2.53 min [M+H]+ 254.3

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo to a reduced volume
  2. customthe residue partitioned between EtOAc and H2O
  3. dry with materialThe organic phase was dried (Na2SO4)
  4. concentrationconcentrated in vacuo
  5. customThe resulting residue was purified by column chromatography (Si—PCC, MeOH:EtOAc, 0-10%)

出典と根拠

ORDレコード
ord-7a64218cf4974ebea079eeb66bf79805
出典データセット
uspto-grants-2013_03
特許番号
US08394796B2

反応ノート

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