Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 1168411생성일: 2026년 10월 25일
Sodium Carbonate → alpha-(4-tert-Butylphenyl)-beta-[(methylthio)carbonyloxy]-beta-(2-trifluoromethylphenyl)acrylonitrile
https://huagongshe.com/reaction/1168411
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | Methyl 3-chlorothiophene-2-carboxylate | HCID 2777566 | — |
| 반응물 | alpha-(4-Tert-butylphenyl)-beta-hydroxy-beta-(2-trifluoromethylphenyl)acrylonitrile | HCID 70026415 | — |
| 용매 | Methyl Ethyl Ketone | HCID 6569 | — |
| 생성물 | alpha-(4-tert-Butylphenyl)-beta-[(methylthio)carbonyloxy]-beta-(2-trifluoromethylphenyl)acrylonitrile | HCID 86759172 | 98.2% |
반응 단계
A mixture comprising 5.0 g of α-(4-tert-butylphenyl)-β-hydroxy-β-(2-trifluoromethylphenyl)acrylonitrile, 1.5 g of sodium carbonate and 30 ml of methyl ethyl ketone, was heated to 70° C., and a mixture comprising 2.1 g of methyl chlorothiolformate and 10 ml of methyl ethyl ketone, was dropwise added over a period of 10 minutes. After completion of the dropwise addition, the reaction was carried out for 30 minutes at a temperature of from 70 to 75° C. The reaction mixture was cooled, and then an inorganic salt was filtered off. The cake was washed with 20 ml of methyl ethyl ketone. Methyl ethyl ketone in the filtrate was distilled off, and to the residue, 50 ml of an isoparaffin type hydrocarbon (tradename: ISOPAR G, manufactured by EXXON CHEMICAL) was added, followed by heating for dissolution, and the solution was left to cool to room temperature. Precipitated crystals were collected by filtration, and the cake was washed with 10 ml of ISOPAR G (tradename) and then dried at 65° C. for 12 hours to obtain 4.9 g of the desired product (isomer ratio 2:98). The HPLC conditions for the analysis of this product were as follows. Further, the NMR spectrum data of this product were the same as in Preparation Example 4.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US06624179B1 |
|---|
| 출처 데이터셋 | uspto-grants-2003_09 |
|---|
| ORD ID | ord-8caf893b6c134ee3b8af7c0b74bc5a2d |
|---|
| 출처 메모 | uspto-grants-2003_09 |
|---|