참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Hexamethyldisilazane | HCID 13838 | — |
| 반응물 | (4-Chlorophenyl)acetic acid | HCID 15880 | — |
| 반응물 | Methyl 2,4-dichlorobenzoate | HCID 37055 | — |
| 반응물 | Sodium | HCID 5360545 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2-(4-Chlorophenyl)-1-(2,4-dichlorophenyl)ethan-1-one | HCID 21984867 | 62.2% |
반응 단계
420 ml of a 2M solution of the sodium salt of hexamethyldisilazane in THF are cooled to −60° C. under a nitrogen atmosphere, 350 ml of THF are added, then, dropwise, a solution of 57.6 g of 4-chlorophenylacetic acid in 70 ml of THF is added and the mixture is left stirring at −60° C. for one hour. 66 g of methyl 2,4-dichlorobenzoate are subsequently added dropwise at −60° C., the mixture is left stirring at −60° C. for 40 minutes and then the temperature is allowed to rise to 0° C. The reaction mixture is poured onto an ice/1 liter of 2N HCl mixture and extracted with ether, the organic phase is dried over Na2SO4, the solvent is concentrated under vacuum to a volume of 150 ml, 200 ml of pentane are added and the crystalline product formed is filtered off. 60 g of the expected compound are obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07589120B2 |
|---|
| 출처 데이터셋 | uspto-grants-2009_09 |
|---|
| ORD ID | ord-64d675e194034178825574bb6bd7d65c |
|---|
| 출처 메모 | uspto-grants-2009_09 |
|---|