Phosphorus oxychloride → Ethyl 4-chloro-5H-pyrrolo[3,2-d]pyrimidine-7-carboxylate
反応式
[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]参加物
4
反応条件
- 温度
- 105 °C
実験手順
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.
後処理
- temperatureThe reaction mixture was cooled
- filtrationthe resulting precipitate was collected by filtration
- washrinsed with EtOAc and Et2O
- customdried under vacuum
出典と根拠
- ORDレコード
- ord-545997e8ed514a9aa7a354ff36f76649
- 出典データセット
- uspto-grants-2011_03
- 特許番号
- US07902204B2
反応ノート
読み込み中…