참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1,4-Dioxane | HCID 31275 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | Phenyl N-(4-(4-(4-methoxyphenyl)piperazin-1-yl)phenyl)carbamate | HCID 981607 | — |
| 반응물 | 2-Methyl-2-(methylamino)propanoic acid hydrochloride | HCID 56777132 | — |
| 촉매 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | HCID 21281918 | HCID 21281918 | 84.4% |
반응 단계
A mixture of 23 parts of methyl 2-methylalanine hydrochloride, 55 parts of phenyl [4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]carbamate. 12.45 parts of sodium hydrogen carbonate, 10 parts of N,N-dimethyl-4-pyridinamine and 300 parts of 1,4-dioxane was stirred overnight at reflux temperature. Water was added till saturation. After stirring for another hour at reflux temperature, the mixture was cooled to room temperature. The product was filtered off, washed with water and 2,2'-oxybispropane and purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (98:2 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was crystallized from 4-methyl-2-pentanone. The product was filtered off and dried. yielding 45.33 parts (84.4%) of 3-[4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]-5,5-dimethyl-2,4-imidazolidinedione; mp. 255.0° C. (intermediate 19).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US04791111 |
|---|
| 출처 데이터셋 | uspto-grants-1988_12 |
|---|
| ORD ID | ord-f33d77786e5d45618d70354830331f58 |
|---|
| 출처 메모 | uspto-grants-1988_12 |
|---|
