Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ammonia → Methyl 2-(3,4-dichlorobenzyl)-4-oxo-3,4-dihydroquinazoline-7-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ammonia | HCID 222 | — |
| 반응물 | (3,4-Dichlorophenyl)acetonitrile | HCID 76690 | — |
| 반응물 | Dimethyl aminoterephthalate | HCID 79336 | — |
| 용매 | 1,4-Dioxane hydrochloride | HCID 20443148 | — |
| 생성물 | Methyl 2-(3,4-dichlorobenzyl)-4-oxo-3,4-dihydroquinazoline-7-carboxylate | HCID 136330126 | — |
반응 단계
420 Milligrams of dimethyl aminoterephthalate and 446 mg of 3,4-dichlorophenylacetonitrile were added to 10 mL of 4N hydrogen chloride dioxane solution and stirred for about 2 days. Pouring the reaction mixture into ice, its pH was adjusted to 8-9 with 25% aqueous ammonia. The precipitated crystals were recovered by filtration and washed with water. The crude crystals were dissolved in chloroform-ethyl acetate (1:1) mixed solvent, and after removing the insoluble matter by filtration, the remaining solution was concentrated. The residue was purified on silica gel column chromatography (hexane:ethyl acetate=4:1) to provide 253 mg of the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08101624B2 |
| 출처 데이터셋 | uspto-grants-2012_01 |
| ORD ID | ord-5444c3375e774297a36f0e4c0ad68e6b |
| 출처 메모 | uspto-grants-2012_01 |