Diethyl Ether → N-Benzoyl-N-methylbenzamide

온도

115 °C

A pressure vessel (Fisher-Porter bottle) equipped with a Teflon coated stir bar, a gas inlet, a pressure gauge, and a pressure release valve was charged with N-methylbenzamide (242 mg, 1.79 mmol), iodobenzene (200 μl, 1.29 mmol), PdCl2L2 (76 mg, 0.107 mmol), triphenylphosphine (56 mg, 0.214 mmol) and DMAc (3.4 ml) and heated (115° C.) under one atmosphere of CO until the reactants had dissolved. DBU (320 μl, 2.14 mmol) was then introduced into the reaction mixture and the reactor charged to 40 psi with CO. After 23 hours, the reactor was cooled to room temperature, depressurized, and the reaction mixture diluted (50 ml) with ether and extracted (3×50 ml) with water. The ether layer was dried over MgSO4 and concentrated to give a red oil which was chromatographed on silica gel (2:1, hexane:ethyl acetate) to give 30 mg product (7%).

1. customA pressure vessel (Fisher-Porter bottle) equipped with a Teflon coated stir bar, a gas inlet
2. dissolutionhad dissolved
3. additionthe reactor charged to 40 psi with CO
4. temperaturethe reactor was cooled to room temperature
5. extractionextracted (3×50 ml) with water
6. dry with materialThe ether layer was dried over MgSO4
7. concentrationconcentrated
8. customto give a red oil which
9. customwas chromatographed on silica gel (2:1, hexane:ethyl acetate)

ORD 기록

ord-e708f93a4dfb46e5b3d387e9f7d32c58

출처 데이터셋

uspto-grants-1990_06

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US04933466