HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 20535104, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Propionyl chloride | HCID 62324 | — |
| Reactant | HCID 20535125 | HCID 20535125 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 20535104 | HCID 20535104 | — |
Reaction Steps
5 g. of 7-amino-5-diallylamino-2H-[1,2,4]oxadiazolo[2,3-a]-s-triazin-2-one are suspended in 80 ml. of methylene chloride and 5 ml. of triethylamine. 2.2 ml. of propionyl chloride in 20 ml. of methylene chloride are added dropwise at 0° C. The mixture is stirred for 90 minutes, then diluted with water, adjusted to pH 4 and extracted with methylene chloride. The combined organic extracts are dried over magnesium sulfate and evaporated under reduced pressure. The residue is chromatographed over silica gel using chloroform for the elution. Recrystallization from methylene chloride and diethyl ether yields pure N-{5-diallylamino-2-oxo-2H-[1,2,4]oxadiazolo[2,3-a]-s-triazin-7-yl}propionamide having a melting point of 157°-159° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04276417 |
| Source dataset | uspto-grants-1981_06 |
| ORD ID | ord-b0ef8485956349efab2c1a77df5d4b23 |
| Source note | uspto-grants-1981_06 |