Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → Methyl 4-[2-(4-bromobenzamido)ethoxy]benzoate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Ethyl chloroformate | HCID 10928 | — |
| 반응물 | 4-Bromobenzoic acid | HCID 11464 | — |
| 반응물 | Methyl 4-(2-aminoethoxy)benzoate | HCID 14097616 | — |
| 용매 | Chloroform | HCID 6212 | — |
| 생성물 | Methyl 4-[2-(4-bromobenzamido)ethoxy]benzoate | HCID 14097618 | 56.7% |
반응 단계
p-Bromobenzoic acid (6 g) and 3.35 g of triethylamine were dissolved in 80 ml of chloroform, the mixture was cooled at 0°-5° C. with stirring, and 3.26 g of ethyl chlorocarbonate was dropped thereinto. The mixture was stirred at the same temperature for 30 minutes, 5.86 g of methyl 4-(2-aminoethoxy)benzoate was added, and the mixture was stirred for 7 hours more. The reaction solution was washed with 10% hydrochloric acid, saturated potassium carbonate solution, and with water, dried with anhydrous magnesium sulphate, concentrated in vacuo, the residue was crystallised with n-hexane, and 8.5 g of crystals obtained were recrystallised from ethyl acetate to give 6.4 g of the product, m.p. 134°-136° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04831055 |
| 출처 데이터셋 | uspto-grants-1989_05 |
| ORD ID | ord-d862fe292fbb498f8de8139483112ffd |
| 출처 메모 | uspto-grants-1989_05 |