Diisopropylethylamine → HCID 178461592, 화합물

HRID 1922860노트

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HRID 1922860 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.[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

참가 물질

4

반응물 3

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

생성물 1

HCID 178461592HCID 178461592, 화합물수율 31.2%

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온도
80 °C

실험 절차

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

후처리

  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%)

출처 및 근거

ORD 기록
ord-912f5c96cd85468ab1a649ed76594103
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08173650B2

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