Tert-Butylamine → t-Butylaminodimethylsilylchloride

Me2SiCl2 (151.50 g, 1.17 moles) was stirred in pentane (2 L) as N(C2H5)3 (119.62 g, 1.18 moles) was added slowly. t-Butylamine (85.85 g, 1.17 moles) in pentane (100 mL) was then added dropwise and the reaction allowed to stir at room temperature for 16 hours. After the reaction period the mixture was filtered and concentrated to 600 mL at which time more salts began to precipitate. The mixture was then refiltered and concentrated to 250 mL and then transferred to a 250 mL roundbottom flask equipped with a microdistillation apparatus and a thermometer. Distillation was performed until the reflux temperature reached 50° C. The clear, colorless liquid remaining was then determined to be pure by NMR and the yield to be essentially quantitative.

1. additionwas added slowly
2. customAfter the reaction period the mixture
3. filtrationwas filtered
4. concentrationconcentrated to 600 mL at which time more salts
5. customto precipitate
6. concentrationconcentrated to 250 mL
7. customtransferred to a 250 mL roundbottom flask
8. customequipped with a microdistillation apparatus
9. distillationDistillation
10. customreached 50° C
11. customthe yield

ORD record

ord-33633c0c914c47e8a04d6a524be0ee63

Source dataset

uspto-grants-2000_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06015868