참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Bromine | HCID 24408 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | 2,6-Dichloro-4'-methoxy-2'-methyl-benzophenone | HCID 54505258 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 5'-Bromo-2,6-dichloro-4'-methoxy-2'-methyl-benzophenone | HCID 54309764 | — |
반응 단계
A solution of bromine (0.25 ml in 3 ml of trichloromethane) is added dropwise to a stirred solution of 2,6-Dichloro-4'-methoxy-2'-methyl-benzophenone (1.5 g; 5 mmol in 5 ml of trichloromethane), followed by 15 minutes of stirring at 20° C. The mixture is shaken with water, sodium hydrogencarbonate solution and water. The organic phase is dried and evaporated. The residue is purified by chromatography (flash column filled with 30 g of silicagel, elution with petrolether/ethylacetate changing from 20:1 to 9:1, 8:2, 7:3 (v/v). After evaporation, the residue crystallises when treated with petrolether/toluene to give white crystalls (0.45 g; 24% y); mp. 159° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05773663 |
|---|
| 출처 데이터셋 | uspto-grants-1998_06 |
|---|
| ORD ID | ord-7fd439dce145453abb5a774147ffde94 |
|---|
| 출처 메모 | uspto-grants-1998_06 |
|---|