Methyl acetoacetate → Methyl 3-tetrahydropyrrolyl-2-butenoate
반응식
[C:1]([O:7][CH3:8])(=[O:6])[CH2:2][C:3]([CH3:5])=O.[NH:9]1[CH2:13][CH2:12][CH2:11][CH2:10]1>C1(C)C=CC=CC=1.O.C1(C)C=CC(S(O)(=O)=O)=CC=1>[NH:9]1[CH2:13][CH2:12][CH2:11][CH:10]1[C:3]([CH3:5])=[CH:2][C:1]([O:7][CH3:8])=[O:6]참가 물질
5
반응 조건
- 온도
- 140 °C
실험 절차
Methyl acetoacetate (20 g, 172.23 mmol) was dissolved in 250 mL of toluene, and then pyrrolidine (43 ml, 516.70 mmol) and p-toluenesulfonic acid hydrate (about 100 mg) were added dropwise. After installing a Dean-Stark separator to the reactor, the reaction mixture was refluxed 140° C. for two days, and then solvent was removed by concentrating the resulting mixture under a reduced pressure, thereby to obtain the desired product (29 g, 99%).
후처리
- customsolvent was removed
- concentrationby concentrating the resulting mixture under a reduced pressure
출처 및 근거
- ORD 기록
- ord-8ef35b9c9c5c40bcabb7b408e1cb86f0
- 출처 데이터셋
- uspto-grants-2006_08
- 특허 번호
- US07094908B2
반응 노트
불러오는 중…