Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → Ethyl (+/-)-[2-(3',4'-dihydro-2'-hydroxyspiro-[cyclopentane-1,1'(2'H)-napthalen]-2'-yl)ethyl]-carbamate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Ethyl chloroformate | HCID 10928 | — |
| 반응물 | (+/-)-2'-(2-Aminoethyl)-3',4'-dihydrospiro[cyclopentane-1,1'(2'H)-napthalen]-2'-ol | HCID 19983233 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | Ethyl (+/-)-[2-(3',4'-dihydro-2'-hydroxyspiro-[cyclopentane-1,1'(2'H)-napthalen]-2'-yl)ethyl]-carbamate | HCID 86745264 | 98% |
반응 단계
A solution of the product from Example 9 (1.05 g, 4.28 mmol) and triethylamine (0.44 g, 4.35 mmol) in 10 mL of CH2Cl2 was cooled to 0° C. and ethyl chloroformate (0.47 g, 4.33 mmol) in 5 mL CH2Cl2 was added dropwise. The reaction was warmed to room temperature and washed with water. The aqueous phase was extracted with CH2Cl2 (3×20 mL) and the combined organic extracts were dried (MgSO4), filtered and concentrated. The residue was purified by chromatography (silica gel, 1:1 heptane/ethyl acetate) to give the title compound (1.33 g, 98%) as an oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05070093 |
| 출처 데이터셋 | uspto-grants-1991_12 |
| ORD ID | ord-0edee85f3a33489abf2d2811f9d81dc3 |
| 출처 메모 | uspto-grants-1991_12 |