참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Benzylamine | HCID 7504 | — |
| 반응물 | Phosphorus oxychloride | HCID 24813 | — |
| 반응물 | 6-Nitro-2,4(1H,3H)-quinazolinedione | HCID 816982 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 2-Chloro-4-benzylamino-6-nitroquinazoline | HCID 18326533 | — |
반응 단계
To 367 mg (1.77 mmol) of 6-nitroquinazoline-2,4 (1H,3H)-dione was added 15.13 g (98.70 mmol) of phosphorus oxychloride to effect reaction in the same manner as in Example 10. Next, to the reaction mixture was added dropwise 379 mg (3.54 mmol) of benzylamine under ice cooling, and the resulting mixture was stirred under ice cooling for 2 hours. Water was added to the reaction mixture, and crystals thus precipitated were filtered out to obtain 2-chloro-4-benzylamino-6-nitroquinazoline. To this was added 761 mg (13.33 mmol) of allylamine, and the resulting mixture was stirred at room temperature for 2.5 hours. Water was added to the reaction mixture, followed by extraction with ethyl acetate, washing with brine and drying over anhydrous sodium sulfate. After the solvent was distilled off, the residue was purified by a silica gel column to give 224 mg (yield: 56.8%) of the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US06339089B2 |
|---|
| 출처 데이터셋 | uspto-grants-2002_01 |
|---|
| ORD ID | ord-141652116b1644c7a1ce2bea9d19db00 |
|---|
| 출처 메모 | uspto-grants-2002_01 |
|---|