Ethylenediamine → P-Cymene

To mixture of ethylenediamine (525 mmol, 31.6 g, 35.2 ml), anhydrous FeCl3 (0,964 mmol, 0.16 g) and sodium (145 mmol, 3.34 g) was heated to about 50° C. under N2. After sodium dissolution had started, as evidenced by hydrogen evolution and formation of a dark solution, α-limonene (742 mmol, 101 g, 120 ml), certified as derived from biomass (obtained from Sigma-Aldrich (St. Louis, Mo.), was added dropwise into the mixture and the mixture heated to 100° C. The mixture was heated at 100° C. for 8 h. The mixture was then cooled down and diluted with water (300 ml) and extracted two times with dichloro methane (DCM) (300 ml). The organic layers were dried over magnesium sulfate and concentrated using a rotary evaporator obtaining the crude para-cymene product. Yield: 99% (purity 99%)

1. additionwas added dropwise into the mixture
2. temperaturethe mixture heated to 100° C
3. temperatureThe mixture was heated at 100° C. for 8 h
4. temperatureThe mixture was then cooled down
5. extractionextracted two times with dichloro methane (DCM) (300 ml)
6. dry with materialThe organic layers were dried over magnesium sulfate
7. concentrationconcentrated
8. customa rotary evaporator

ORD 기록

ord-cc376bf4aa5a4a1d84f3697d70c2c472

출처 데이터셋

uspto-grants-2016_05

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US09328045B2