Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethylamine → (1R,2R)-N1,N1-Dimethylcyclohexane-1,2-diamine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethylamine | HCID 674 | — |
| 반응물 | Ethanol | HCID 702 | — |
| 반응물 | 7-Azabicyclo[4.1.0]heptane | HCID 549240 | — |
| 촉매 | Palladium | HCID 23938 | — |
| 생성물 | (1R,2R)-N1,N1-Dimethylcyclohexane-1,2-diamine | HCID 11275066 | — |
반응 단계
A solution of the benzylamino compound is hydrogenated in two batches, each containing 30.5 g. (0.131 mole), 175 ml. EtOH, 3.4 g Pd-C and 56.5 g. (0.394 mole) of 70% HClO4, at initial pressure of 51.5 p.s.i. for 19 hours. The two reduced batches are combined, filtered through Celite, and evaporated in vacuo at 45°. The residue is cooled in ice, basified with 40% KOH to pH 11. The resulting thick suspension is extracted with ether (5 × 200 ml.), the ether extract dried (MgSO4) and evaporated through a 9" Vigreux. The residue is distilled at 13 mm to give 32.5 g. (87% yield), b.p. 77°-78.5°. ir and nmr are identical to those of the sample prepared by the reaction of 7-azabicyclo[4.1.0]heptane with dimethylamine (Procedure I, Part C).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04145435 |
| 출처 데이터셋 | uspto-grants-1979_03 |
| ORD ID | ord-54680085629644229891d96f24710c80 |
| 출처 메모 | uspto-grants-1979_03 |