Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dichloromethane → HCID 14156369, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dichloromethane | HCID 6344 | — |
| 반응물 | O-Xylene | HCID 7237 | — |
| 반응물 | 1,3-Cyclopentanedicarboxylic anhydride | HCID 239799 | — |
| 반응물 | 4-[4-(3-Chlorophenyl)piperazin-1-yl]butan-1-amine | HCID 12840704 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | HCID 14156369 | HCID 14156369 | — |
반응 단계
1,3-Cyclopentane dicarboxylic anhydride (2.2 g., 15 mmole) and 4.0 g. (15 mmole) of 1-(4-aminobutyl)-4-(3-chlorophenyl)piperazine were combined in 300 ml. of methylene chloride and stirred for 30 minutes at room temperature. The solvent was replaced with xylene and the mixture was refluxed for 48 hours with water removal via a Dean-Stark trap. The solvent was removed in vacuum and the residue filtered through 75 g. of silica gel with 2% ethanol/chloroform as eluent. The product was concentrated in vacuum and crystallized from 50 ml. of isopropanol with addition of 4N isopropanolic HCl. Recrystallization from ethanol gave 1.6 g. of the title compound as the hydrochloride, quarter hydrate; m.p. 199°-202° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04748240 |
| 출처 데이터셋 | uspto-grants-1988_05 |
| ORD ID | ord-0414f49d39d6428e8394f535d7f0ce73 |
| 출처 메모 | uspto-grants-1988_05 |