참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ammonia | HCID 222 | — |
| 반응물 | Carbamic acid, octyl ester | HCID 16240 | — |
| 반응물 | N,N'-bis(2,2-dimethyl-3-aminopropyl)piperazine | HCID 20031516 | — |
| 용매 | 1-Octanol | HCID 957 | — |
| 생성물 | N,N'-bis(octoxycarbonylaminoneopentyl)piperazine | HCID 20429701 | — |
반응 단계
Agitated in a reaction vessel are 256 parts of N,N'-bis(2,2-dimethyl-3-aminopropyl)piperazine with 400 parts of O-octyl carbamate and 130 parts of n-octanol at a reflux temperature of 190° C.-200° C. for 1 hour while the ammonia is removed by distillation. At that point, an additional 650 parts of n-octanol are allowed to flow into the reaction mixture and the reaction is continued at reflux temperature for 7 hours. Unreacted octanol and O-octylcarbonate are removed by distillation up to a sump temperature of 180° C.-200° C. at 2 millibars. By transcrystallization of the residue from acetone/water, 506 parts of N,N'-bis(octoxycarbonylaminoneopentyl)piperazine, C32H64N4O4 (molecular weight 568), are obtained corresponding with 89 percent of theory relative to N,N'-bis(2,2-dimethyl-3-aminopropyl)piperaxine. The melting point is 66° C.-68° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US04497963 |
|---|
| 출처 데이터셋 | uspto-grants-1985_02 |
|---|
| ORD ID | ord-cbff6c233fa1441c9da0a8759997e908 |
|---|
| 출처 메모 | uspto-grants-1985_02 |
|---|