Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methyl 2-nitroacetate → 5-Dimethylamino-2-nitro-4-[4-chloro-2-nitrophenyl]-2,4-pentadienoic acid methyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methyl 2-nitroacetate | HCID 17206 | — |
| 반응물 | 3-Dimethylamino-2-[4-chloro-2-nitrophenyl]acrolein | HCID 53802900 | — |
| 용매 | Acetic Anhydride | HCID 7918 | — |
| 생성물 | 5-Dimethylamino-2-nitro-4-[4-chloro-2-nitrophenyl]-2,4-pentadienoic acid methyl ester | HCID 54135004 | 89% |
반응 단계
A mixture of 73.1 g (0.29 mol) of the compound of Example 13, 34.0 g (0.29 mol) of methyl nitroacetate and 600 ml of acetic anhydride was stirred and heated at 90°-95° for 45 minutes. The reaction mixture was allowed to cool to room temperature and the crystalline product was collected by filtration. The filtrate was concentrated in vacuo and the residue was slurried with ether (200 ml.) and filtered. The combined materials were washed with ether and dried to give 91.0 g (89%) of red orange crystals, m.p. 193°-197°. Recrystallization from benzenedimethylformamide (6:1,1725 ml) afforded 78.8 g (77%) of product, m.p. 198°-200°.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04256641 |
| 출처 데이터셋 | uspto-grants-1981_03 |
| ORD ID | ord-095bee3a554d4eb387f5578d3b123b6c |
| 출처 메모 | uspto-grants-1981_03 |