HEXANE-1,6-DIYLBIS(METHYLCARBAMIC CHLORIDE) synthesis
- Product Name:HEXANE-1,6-DIYLBIS(METHYLCARBAMIC CHLORIDE)
- CAS Number:99191-71-6
- Molecular formula:C10H18Cl2N2O2
- Molecular Weight:269.17
Yield:99191-71-6 367.8 g
Reaction Conditions:
in toluene at 60;
Steps:
1 Example 1
To the reactor, 2.8 L of toluene and 758 g of triphosgene were added in that order.And N,N,N',N'-tetramethylhexyldiamine 400g,Raise the temperature to 60°CTLC detects the reaction of the raw materials.filter,The filtrate is concentrated under reduced pressure,Intermediate 5.3 g of crude product was obtained.To the above crude product was added ethyl acetate/methyl tert-butyl ether mixed solvent 2L.Heat to completely dissolve and filterThe filtrate was slowly cooled to 0°C.Stirring and crystallization,filter,Solids are vacuum dried at 30°C,Obtained Intermediate III Refined Product 367.8g,HPLC purity: 98.75%.
References:
CN107915675,2018,A Location in patent:Paragraph 0007; 0021-0023
