Guanidine → 2-Amino-7-bromoquinazoline
反応式
[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]=1参加物
5
実験手順
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).
後処理
- 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
出典と根拠
- ORDレコード
- ord-0e80b63316c64135a8352b023fccb35d
- 出典データセット
- uspto-grants-2004_12
- 特許番号
- US06831175B2
反応ノート
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