Methylamine → HCID 86643717, compound

Temperature

-10 °C

A three-necked flask in which the internal atmosphere was sufficiently replaced with nitrogen gas was charged with 60 ml of a THF solution containing 0.04 mol of ethylamine in a nitrogen stream. 30 ml of a hexane solution containing 0.04 mol of BuLi was slowly added to the ethylamine solution cooled to −10° C. using a dripping funnel. After the addition, the mixture was gradually heated and reacted at 50° C. for two hours. Another container of which the internal atmosphere was purged with nitrogen was charged with 60 ml of a toluene solution containing 0.02 mol of t-butylethyldimethoxysilane and cooled to −10° C. The above slurry of Li salt of methylamine was slowly added dropwise to the cooled solution under nitrogen seal. After the addition, the mixture was reacted at 50° C. for three hours. The reaction mixture was separated into a solid and a solution by centrifugation. The solid was washed with 20 ml of toluene and added to the solution. The solvent was evaporated from the solution under reduced pressure and the residue was distilled under reduced pressure to obtain bis(methylamino)-t-butylethylsilane. The elementary analysis confirmed that the compound consists of C: 55.01% (55.11%), H: 12.57% (12.72%), and N: 16.25% (16.07%), wherein the percentages of the parentheses are theoretical values.

1. customA three-necked flask in which the internal atmosphere was sufficiently replaced with nitrogen gas
2. additionAfter the addition
3. temperaturethe mixture was gradually heated
4. customreacted at 50° C. for two hours
5. customAnother container of which the internal atmosphere was purged with nitrogen
6. additionwas charged with 60 ml of a toluene solution
7. temperaturecooled to −10° C
8. customseal
9. additionAfter the addition
10. customthe mixture was reacted at 50° C. for three hours
11. customThe reaction mixture was separated into a solid
12. washThe solid was washed with 20 ml of toluene
13. additionadded to the solution
14. customThe solvent was evaporated from the solution under reduced pressure
15. distillationthe residue was distilled under reduced pressure

ORD record

ord-f7035f472e884cb1bf85e5c4024ff7e7

Source dataset

uspto-grants-2014_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08648001B2