Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
2,4-Dioxo-2,4-dihydro-1H-benzo[D][1,3]oxazine-6-carboxylic acid → 4-Amino-3-(methoxycarbonyl)benzoic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 2,4-Dioxo-2,4-dihydro-1H-benzo[D][1,3]oxazine-6-carboxylic acid | HCID 12724728 | — |
| 촉매 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 4-Amino-3-(methoxycarbonyl)benzoic acid | HCID 12724725 | 84% |
반응 단계
150 mg (1.21 mmol) of 4-dimethylaminopyridine are added to 2.5 g (12.1 mmol) of 2,4-dioxo-1,4-dihydro-2H-3,1-benzoxazine-6-carboxylic acid [described in J. Med. Chem., (1981), 24(6), 735-742] in solution in 10 ml of dimethylformamide and 10 ml of methanol, and the mixture is heated at 60° C. for 3 hours. The reaction medium is concentrated under reduced pressure. The residue is taken up in water and extracted with ethyl acetate. The organic phase is washed with a saturated sodium chloride solution, dried over sodium sulphate and concentrated under reduced pressure. The solid obtained is taken up in ethyl acetate, filtered and dried. 1.98 g of a white powder are obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07803811B2 |
| 출처 데이터셋 | uspto-grants-2010_09 |
| ORD ID | ord-3fc290cd34034bd3b0b5c3dc926e1966 |
| 출처 메모 | uspto-grants-2010_09 |