関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Morpholino-1-propanol | HCID 199576 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 反応物 | 7-Fluoro-4-[(3-methylphenyl)-amino]-6-nitroquinazoline | HCID 10542070 | — |
| 反応物 | Dichloromethane ethyl acetate methanol | HCID 21901258 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | Methylenechloride Hexane | HCID 21226440 | — |
| 生成物 | HCID 10526285 | HCID 10526285 | 88% |
反応手順
To a solution of 3-morpholinopropan-1-ol (8.40 mmol, 1.22 g) in THF (40 mL) under N2 was added sodium metal (11.8 mmol, 0.27 g). The resulting suspension was stirred at 20° C. for 2 hours and then cannulated into a solution of 7-fluoro-4-[(3-methyl-phenyl)amino]-6-nitroquinazoline (0.70 g, 2.35 mmol) in THF (30 mL) under N2. The reaction procedure and workup above were followed to give after chromatography on silica gel eluting with MeOH/CH2Cl2/EtOAc (5:45:50) to MeOH/CH2C0.50/EtOAc (3:7:10) 4-[(3-methylphenyl)-amino]-7-[(3-morpholino)propyloxy]-6-nitroquinazoline (0.87 g, 88%) as a yellow powder, mp (CH2Cl2/hexane) 169-170° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06602863B1 |
|---|
| 出典データセット | uspto-grants-2003_08 |
|---|
| ORD ID | ord-4ea7868d374341998b12f231bd3ca726 |
|---|
| 出典メモ | uspto-grants-2003_08 |
|---|
