Ethyl orthoformate → HCID 178468256, compound

A mixture was prepared from 50 g of 5-aminotetrazole, 347 g of triethoxymethane and 500 ml of hexane and this was heated under nitrogen so that distillation took place at a moderate rate (head temperature about 60°-68° C.). Distillate was collected over a period of 6 hours with hexane being replaced in the reaction mixture as necessary. The mixture was then cooled to room temperature and the fine white needles that formed were collected by filtration, washed with hexane and vacuum oven dried with heating to give 5-(ethoxymethyleneamino)tetrazole. This material hydrolyzes rapidly on exposure to atmospheric moisture so that it should be used promptly for any further reactions desired or it should be stored using appropriate conditions.

1. temperaturethis was heated under nitrogen so that distillation
2. customat a moderate rate (head temperature about 60°-68° C.)
3. distillationDistillate was collected over a period of 6 hours with hexane being
4. customthe fine white needles that formed
5. filtrationwere collected by filtration
6. washwashed with hexane and vacuum oven
7. customdried
8. temperaturewith heating

ORD record

ord-f20d34c74feb498e80ae0a37618d9ac6

Source dataset

uspto-grants-1987_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04644065