Formamide → 3-Amino-2,2,4,4-tetramethylthietane

Temperatur

175 °C

Formamide (4.0 g, 89 mmol), 2,2,4,4-tetramethyl-3-oxothietane (1.0 g, 6933 mmol) and boric acid (100 mg) were combined in a Teflon lined Parr bomb which was heated for 15 hours in a 175° C. oil bath. The reaction was cooled and the light brown mixture taken up in water (40 ml). The aqueous solution was extracted with methylene chloride (4×20 ml) and the combined extracts dried (MgSO4) and evaporated under reduced pressure to a light brown oil (1.02 g). The residue was hydrolyzed and the hydrolyzate worked up according to the procedure of Example 1 to give the title product 650 mg (65%), verified by its 1H-NMR spectrum.

1. temperatureThe reaction was cooled
2. extractionThe aqueous solution was extracted with methylene chloride (4×20 ml)
3. dry with materialthe combined extracts dried (MgSO4)
4. customevaporated under reduced pressure to a light brown oil (1.02 g)

ORD-Eintrag

ord-ae832359f86a4740a2a0aded07d8bfb6

Quelldatensatz

uspto-grants-1989_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US04851548