참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Phosphoric Acid | HCID 1004 | — |
| 반응물 | Dimethyl Sulfate | HCID 6497 | — |
| 반응물 | Sodium alpha-[4-(4-Trifluoromethylphenoxy)phenoxy]propionate | HCID 23675546 | — |
| 용매 | O-Xylene | HCID 7237 | — |
| 생성물 | Trifop-methyl | HCID 94586 | — |
반응 단계
63 g of dimethyl sulfate are added within 5 minutes and at 130° C. to 348 g of anhydrous sodium-2-[4'-(4"-trifluoromethyl-phenoxy)-phenoxy]-propionate, suspended in 1,000 ml of xylene. After the addition, stirring of the mixture is continued for 1 hour, the mixture is cooled at 85° C., at said temperature 200 ml of water and 0.5 ml of H3PO4 are added and, for the separation of the inorganic salts, the mixture is stirred for 10 minutes. After separation of the water phase, the xylene is distilled off. 340 g of methyl-2-[4'-(4"-trifluoromethyl-phenoxy)-phenoxy]-propionate are obtained melting at 142° C. under 0.05 torr. According to gas chromatogram the content of pure final product is 99.4%, the residual content of unreacted acid is 0.6%, which corresponds to a yield of 99.4%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US04252980 |
|---|
| 출처 데이터셋 | uspto-grants-1981_02 |
|---|
| ORD ID | ord-4c4ffb351c7643d1bc21a5c46786903b |
|---|
| 출처 메모 | uspto-grants-1981_02 |
|---|