1,1'-Biphenyl, mixt. with 1,1'-oxybis(benzene) → Ethyl 8-chloro-4-oxo-5-(trifluoromethyl)-1,4-dihydroquinoline-3-carboxylate
반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([F:11])([F:10])[F:9])=[CH:4][C:3]=1[NH:12][CH:13]=[C:14]([C:20](OCC)=[O:21])[C:15]([O:17][CH2:18][CH3:19])=[O:16].C1C=CC(C2C=CC=CC=2)=CC=1.C1C=CC(OC2C=CC=CC=2)=CC=1>>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([F:9])([F:10])[F:11])=[C:4]2[C:3]=1[NH:12][CH:13]=[C:14]([C:15]([O:17][CH2:18][CH3:19])=[O:16])[C:20]2=[O:21]참가 물질
3
반응 조건
- 온도
- 260 °C
실험 절차
Compound 6B (2000 g, 5.468 mol) was introduced into the reactor. Dowtherm (4.000 L) was charged to the reactor and degassed at room temperature overnight with nitrogen purge. It was then stirred and warmed to 260° C. EtOH produced was distilled off. The reaction was monitored and was complete after 5.5 h, the reaction was substantially complete. Heat source was removed and the reaction mixture was cooled to 80° C. and heptane (2.000 L) was charged. The mixture was stirred for 30 min. Heptane (6.000 L) was charged to the stirred mixture and stirring continued overnight. Solids were filtered off and washed with heptane (4.000 L) and dried in a vacuum oven at 50° C. to provide Compound 6A.
후처리
- customdegassed at room temperature overnight with nitrogen
- custompurge
- customEtOH produced
- distillationwas distilled off
- temperatureHeat source
- customwas removed
- temperaturethe reaction mixture was cooled to 80° C.
- additionheptane (2.000 L) was charged
- stirringThe mixture was stirred for 30 min
- additionHeptane (6.000 L) was charged to the stirred mixture
- stirringstirring continued overnight
- filtrationSolids were filtered off
- washwashed with heptane (4.000 L)
- customdried in a vacuum oven at 50° C.
출처 및 근거
- ORD 기록
- ord-ee2099a61dc64bee9f52f1c29dbb03f9
- 출처 데이터셋
- uspto-grants-2014_11
- 특허 번호
- US08884018B2
반응 노트
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