Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ammonium Chloride → Tert-butyl 2-oxo-7-azaspiro[3.5]nonane-7-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | Tert-butyl 1,1-dichloro-2-oxo-7-azaspiro[3.5]nonane-7-carboxylate | HCID 9857764 | — |
| 촉매 | Zinc | HCID 23994 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | Tert-butyl 2-oxo-7-azaspiro[3.5]nonane-7-carboxylate | HCID 11195798 | 80.2% |
반응 단계
106.1 g zinc dust was added to a mixture of 62.5 g tert-butyl 1,1-dichloro-2-oxo-7-azaspiro[3.5]nonane-7-carboxylate and 500 ml saturated ammonium chloride in methanol. The mixture was stirred for 1 hr and 20 min at room temperature and filtered through Celite. The filtrate was evaporated, 1 N hydrochloric acid/ethyl acetate was added thereto, and the organic layer was recovered. The extract was washed with water, saturated sodium bicarbonate and brine, dried over anhydrous magnesium sulfate, and filtered. The filtrate was evaporated, and the resulting residue was subjected to silica gel column chromatography to give 38.9 g of tert-butyl 2-oxo-7-azaspiro[3.5]nonane-7-carboxylate.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06699870B2 |
| 출처 데이터셋 | uspto-grants-2004_03 |
| ORD ID | ord-97e74cb0144947d491a5546620c3a145 |
| 출처 메모 | uspto-grants-2004_03 |