Guanidine → 2-Amino-7-bromoquinazoline
반응식
[Br:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=O)=[C:4](F)[CH:3]=1.[NH2:11][C:12]([NH2:14])=[NH:13].CN(C=O)C>O>[Br:1][C:2]1[CH:3]=[C:4]2[C:5]([CH:6]=[N:11][C:12]([NH2:14])=[N:13]2)=[CH:8][CH:9]=1참가 물질
5
실험 절차
The 4-Bromo-2-fluoro-benzaldehyde (0.61 g, 3 mmol), guanidine (1.05 g, 5.83 mmol) and DMF were heated at 140° C. for 2.5 hours. 50 ml water was added to the mixture. The orange precipitate was filtered and washed with water. The solid was dissolved in 2N HCl. and filtered. The HCl solution was neutralized by ammonia hydroxyl. The off white solid was filtered and dried under vacuum to afforded the desired product (91 mg, 14%). MS (ESI) m/e 224 (M+1)+; 1H NMR (300 MHz, DMSO-D6) δ ppm 7.00 (br. s., 2 H) 7.36 (d, J=8.82 Hz, 1 H) 7.77 (dd, J=9.16, 2.37 Hz, 1 H) 8.05 (d, J=2.37 Hz, 1 H) 9.09 (br. s., 1 H).
후처리
- filtrationThe orange precipitate was filtered
- washwashed with water
- dissolutionThe solid was dissolved in 2N HCl
- filtrationand filtered
- filtrationThe off white solid was filtered
- customdried under vacuum
출처 및 근거
- ORD 기록
- ord-0e80b63316c64135a8352b023fccb35d
- 출처 데이터셋
- uspto-grants-2004_12
- 특허 번호
- US06831175B2
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