Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
2-(1H-imidazol-1-yl)ethanamine → HCID 178477864, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 2-(1H-imidazol-1-yl)ethanamine | HCID 430667 | — |
| 반응물 | 8-Chloro-5,10-dihydro-dibenzo[b,e][1,4]diazepin-11-thione | HCID 12535778 | — |
| 용매 | Glycol monoethyl ether | HCID 8076 | — |
| 생성물 | HCID 178477864 | HCID 178477864 | 57.1% |
반응 단계
A solution of 0.6 g (2.3 mmol) of 8-chloro-5,10-dihydro-dibenzo[b,e][1,4]diazepin-11-thione in 15 mL of 2-ethoxyethanol was treated with 0.6 mL (4.6 mmol) of 1-(2-aminoethyl)imidazole and heated at reflux for 2 days. The solvent was removed under reduced pressure and the residue taken up in EtOAc and washed three times with H2O, then saturated NaHCO3 solution, and saturated NaCl solution. Drying over MgSO4 and removal of the solvent under reduced pressure left the crude product. This was recrystallized from EtOAc/hexane using charcoal to give 0.44 g (57.1% yield) of the product as pale yellow crystals, mp 168-170° C. The structure was confirmed by NMR and mass spectroscopy. (m+H)+ =338.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05919780 |
| 출처 데이터셋 | uspto-grants-1999_07 |
| ORD ID | ord-5b925a6dbad44516b076de80e86a116d |
| 출처 메모 | uspto-grants-1999_07 |