Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
tert-Butoxy bis(dimethylamino)methane → 1-Tert-butyl 3-ethyl 5-((dimethylamino)methylene)-4-oxopiperidine-1,3-dicarboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | tert-Butoxy bis(dimethylamino)methane | HCID 79885 | — |
| 반응물 | 1-(1,1-Dimethylethyl) 3-ethyl 4-oxo-1,3-piperidinedicarboxylate | HCID 6420876 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 1-Tert-butyl 3-ethyl 5-((dimethylamino)methylene)-4-oxopiperidine-1,3-dicarboxylate | HCID 68465860 | — |
반응 단계
To a solution of 2b (272 mg, 1.00 mmol) in dry toluene (4.0 mL) was added Bredereck's reagent (183 mg, 1.05 mmol) dropwise over 2 minutes. The mixture stirred at rt for 1 h and heated to 60° C. for 24 h. The mixture was concentrated and the residue purified on a SiO2 column (CH2Cl2, 50% EtOAc-hexanes then EtOAc for elution) to give a viscous oil. The oil was dissolved in 50% Et2O-hexanes and concentrated to give the title compound 3b as a waxy white solid; 243 mg, 74%. This material was used immediately without further purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07781474B2 |
| 출처 데이터셋 | uspto-grants-2010_08 |
| ORD ID | ord-d2a4d8a3dc9349719342c7abedc32bd7 |
| 출처 메모 | uspto-grants-2010_08 |