참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Phosphorus oxychloride | HCID 24813 | — |
| 반응물 | 7-Methyl-4(3H)-quinazolinone | HCID 135452533 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 4-Chloro-7-methylquinazoline | HCID 21942014 | — |
반응 단계
To a solution of 7-methyl-3H-quinazolin-4-one (10.6 g, 69 mmol) in toluene (350 mL) is added triethylamine (17.5 g, 173 mmol) followed by phosphorous oxychloride (12.3 g, 80 mmol). The resulting solution is heated to 80° C. After 4 hours, the solution is cooled to ambient temperature. The reaction mixture is poured into 500 mL of water. The layers are separated and the organic layer is washed with H2O, saturated NaHCO3, and saturated NaCl, dried over MgSO4, filtered and concentrated. The resulting crude product is purified by recrystallization from EtOAc. The title compound is obtained as a white solid (10 g, 56 mmol). 1H NMR (CDCl3, 300 MHz) δ9.02 (s, 1H), 8.16 (d, 1H), 7.87 (s, 1H), 7.55 (d, 1H), 2.62 (s, 3H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07612075B2 |
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| 출처 데이터셋 | uspto-grants-2009_11 |
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| ORD ID | ord-c99e29bc5508448993712c48483b72e9 |
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| 출처 메모 | uspto-grants-2009_11 |
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