반응식
[NH2:1][C:2]1[N:10]=[C:9]2[C:5]([NH:6][CH:7]=[N:8]2)=[C:4](Cl)[N:3]=1.[OH-].[Na+].[CH2:14]([OH:21])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1>>[NH2:1][C:2]1[N:10]=[C:9]2[C:5]([NH:6][CH:7]=[N:8]2)=[C:4]([O:21][CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[N:3]=1참가 물질
4
반응 조건
- 온도
- 100 °C
실험 절차
To a 500 mL 3 neck round bottom flask equipped with a magnetic stirrer, temperature probe and nitrogen inlet was added 2-amino-6-chloropurine (20 g), sodium hyroxide (28 g) and benzyl alcohol (200 mL). The mixture was stirred for 20 minutes and then heated at 100° C. for 2-3 hours. The reaction mixture was then cooled to room temperature and partitioned between methyl t-butyl ether (300 mL) and water (300 mL). The aqueous layer was separated and the pH was adjusted to 7-8 with 6 M HCl. The resulting solid was filtered, washed with water (50 mL) and dried under vacuum at 50° C. for 20 hours to provide the desired product as a pale yellow solid (24.3 g).
후처리
- temperatureThe reaction mixture was then cooled to room temperature
- custompartitioned between methyl t-butyl ether (300 mL) and water (300 mL)
- customThe aqueous layer was separated
- filtrationThe resulting solid was filtered
- washwashed with water (50 mL)
- customdried under vacuum at 50° C. for 20 hours
출처 및 근거
- ORD 기록
- ord-8a890804f98b4dab913201802d86eee2
- 출처 데이터셋
- uspto-grants-2001_02
- 특허 번호
- US06184376B2
연결된 노트
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