반응식
[C:1]([C:5](O)=O)([F:4])([F:3])[F:2].C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.CCN(CC)CC.[CH:34]1([C:37]2[CH:42]=[CH:41][C:40]([N+:43]([O-:45])=[O:44])=[CH:39][C:38]=2[NH2:46])[CH2:36][CH2:35]1.C(Cl)(Cl)(Cl)[Cl:48]>>[Cl:48]/[C:5](=[N:46]\[C:38]1[CH:39]=[C:40]([N+:43]([O-:45])=[O:44])[CH:41]=[CH:42][C:37]=1[CH:34]1[CH2:36][CH2:35]1)/[C:1]([F:4])([F:3])[F:2]참가 물질
6
실험 절차
A mixture of CF3CO2H (0.98 mL, 12.65 mmol, 0.9 eq), PPh3 (9.21 g, 35.13 mmol, 2.5 eq) and Et3N (1.96 mL, 14.05 mmol, 1.0 eq), in 25 mL CCl4 was stirred at 0° C. for 10 minutes. 2-Cyclopropyl-5-nitrobenzeneamine (2.50 g, 14.05 mmol, 1.0 eq) was then added to the reaction mixture and the mixture was heated to reflux for 12 hours. Solvent was removed under reduced pressure and the residue was purified by column chromatography, eluting with n-hexane: ethyl acetate (10:1), giving the (Z)—N-(1-chloro-2,2,2-trifluoroethylidene)-2-cyclopropyl-5-nitrobenzenamine intermediate in semi pure form as a light yellow solid. This compound was taken to the next step with out further purification.
후처리
- temperaturethe mixture was heated
- temperatureto reflux for 12 hours
- customSolvent was removed under reduced pressure
- customthe residue was purified by column chromatography
- washeluting with n-hexane: ethyl acetate (10:1)
출처 및 근거
- ORD 기록
- ord-6c56f8dcb16c4d60bd56a82361a88739
- 출처 데이터셋
- uspto-grants-2015_11
- 특허 번호
- US09181222B2
연결된 노트
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