Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium Carbonate → Methyl 6-amino-2-methyl-3-nitrobenzoate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | 6-Methylanthranilic acid | HCID 151210 | — |
| 반응물 | 5-Methyl-6-nitro-1H-benzo[d][1,3]oxazine-2,4-dione | HCID 21901154 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | Methyl 6-amino-2-methyl-3-nitrobenzoate | HCID 15334532 | 87.1% |
반응 단계
5-Methyl-6-nitro-1H-benzo[d][1,3]oxazine-2,4-dione (8 g, 36.0 mmol) prepared from 2-Amino-6-methyl-benzoic acid (Aldrich) as described by Abood, N. A., et al. (1997) Bioorganic & Med. Chem. Lett. 7: 2105-2108 and sodium carbonate (3.82, 36.0 mmol) were stirred in methanol (180 mL, 0.1 M) at 0° C. for 0.5 hours and then at ambient temperature for 3 hours. Strongly acidic ion-exchange resin (Dowex® 50 WX4-200) was added until neutral pH and the solution was filtered. The solvent was removed under reduced pressure and silica gel chromatography (60:40 hexane/ethyl acetate) afforded Intermediate 1(a) (6.59 g) in 87% yield.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06967198B2 |
| 출처 데이터셋 | uspto-grants-2005_11 |
| ORD ID | ord-7492f88a602345f280d558575cc10673 |
| 출처 메모 | uspto-grants-2005_11 |