Allylamine → N-((trimethylsilyl)methyl)prop-2-en-1-amine

温度

70 °C

To 118 mL (1.57 mol) of allylamine warmed at 40° C. in an inert atmosphere was very slowly added 100 mL (0.72 mol) of chloromethyl trimethylsilane (approximate rate of 1 mL/min). The reaction mixture was slowly warmed to 70° C. and stirred for 24 h. The reaction mixture was cooled to 0° C. and to it was added water to break up the gel and then 300 mL of 2N NaOH solution. The reaction mixture was extracted with ether. The combined organic fractions were washed with 500 mL of sat'd NaCl solution, dried over Na2SO4, filtered and the filtrate was concentrated. The residue was purified by distillation (bp 80-84° C. @ 100 torr) to give 75 g of the title compound.

1. temperatureThe reaction mixture was cooled to 0° C. and to it
2. extractionThe reaction mixture was extracted with ether
3. washThe combined organic fractions were washed with 500 mL of sat'd NaCl solution
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationthe filtrate was concentrated
7. distillationThe residue was purified by distillation (bp 80-84° C. @ 100 torr)

ORDレコード

ord-3f22cc22fc3945dabe3dbc31a0321663

出典データセット

uspto-grants-2002_03

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06362201B1