Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium hydride → 5-amino-1-(2-chlorobenzyl)-7-(trifluoromethyl)-1,3-dihydro-2H-benzimidazol-2-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | Ethyl 2-chlorobenzyl[2,4-diamino-6-(trifluoromethyl)phenyl]carbamate | HCID 20827733 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | 5-amino-1-(2-chlorobenzyl)-7-(trifluoromethyl)-1,3-dihydro-2H-benzimidazol-2-one | HCID 22327374 | 61% |
반응 단계
Ethyl 2-chlorobenzyl[2,4-diamino-6-(trifluoromethyl)phenyl]carbamate (85.6 mg) was dissolved in ethanol (10 ml), and to the solution was added sodium hydride (17.7 mg). The reaction mixture was heated at reflux for 24 hours. After allowing to cool, to the reaction mixture was added saturated aqueous sodium bicarbonate solution, and the mixture was extracted 4 times with chloroform. The organic layer was washed with saturated brine, dried over anhydrous sodium sulfate, and concentrated in vacuo. The resultant residue was purified by preparative TLC (2 mm, 20×20 cm, CHCl3-methanol=5:1) to give the title compound (46.0 mg).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06939887B2 |
| 출처 데이터셋 | uspto-grants-2005_09 |
| ORD ID | ord-5f92d9fbca3e4bc7aa638c6258538e88 |
| 출처 메모 | uspto-grants-2005_09 |