Phosphorus oxychloride → Ethyl 4-chloro-5H-pyrrolo[3,2-d]pyrimidine-7-carboxylate
반응식
[CH2:1]([O:3][C:4]([C:6]1[C:10]2[N:11]=[CH:12][N:13]=[C:14](O)[C:9]=2[NH:8][CH:7]=1)=[O:5])[CH3:2].O=P(Cl)(Cl)[Cl:18]>CCOCC>[CH2:1]([O:3][C:4]([C:6]1[C:10]2[N:11]=[CH:12][N:13]=[C:14]([Cl:18])[C:9]=2[NH:8][CH:7]=1)=[O:5])[CH3:2]참가 물질
4
반응 조건
- 온도
- 105 °C
실험 절차
4,6-Diazaindole 4 (2.74 g, 13.2 mmol) was slurried in POCl3 (37 mL, 400 mmol) and heated at 105° C. for 3.5 h. The reaction mixture was cooled, diluted with Et2O (150 mL) and the resulting precipitate was collected by filtration, rinsed with EtOAc and Et2O and dried under vacuum to yield 7-chloro-4,6-diazaindole 5 (2.48 g, 11.0 mmol, 83%) as a yellow powder which was used without further purification.
후처리
- temperatureThe reaction mixture was cooled
- filtrationthe resulting precipitate was collected by filtration
- washrinsed with EtOAc and Et2O
- customdried under vacuum
출처 및 근거
- ORD 기록
- ord-545997e8ed514a9aa7a354ff36f76649
- 출처 데이터셋
- uspto-grants-2011_03
- 특허 번호
- US07902204B2
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