Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Chloroacetyl chloride → DL-Alanine, N-(chloroacetyl)-N-(2,6-dimethylphenyl)-, methyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Chloroacetyl chloride | HCID 6577 | — |
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | Methyl N-(2,6-dimethylphenyl)-DL-alaninate | HCID 94555 | — |
| 용매 | Benzene | HCID 241 | — |
| 생성물 | DL-Alanine, N-(chloroacetyl)-N-(2,6-dimethylphenyl)-, methyl ester | HCID 6452743 | — |
반응 단계
990.3 g (= 4.76 g-moles) of α-(2,6-dimethylanilino)-propionic acid methyl ester is mixed with 605 g (= 5.7 g-moles) of sodium carbonate in 2.5 liters of benzene (absolute). An amount of 455 ml (= 5.7 g-moles) of monochloroacetyl chloride is then added dropwise and sufficiently slowly to ensure that a temperature of 30°-35° in the reaction mixture is not exceeded. After stirring has been maintained overnight at room temperature, the mixture is filtered off, and the filtrate concentrated in a rotary evaporator at ca. 50°. The resulting residue is recrystallised from ligroin (boiling range 65°-90° ). The yield obtained is 1132 g (= 83.8% of theory) of final product, M.P. 92°-94° (compound No. 3).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04034108 |
| 출처 데이터셋 | uspto-grants-1977_07 |
| ORD ID | ord-70276b4e689f49109141655fea5c0385 |
| 출처 메모 | uspto-grants-1977_07 |