HuagongsheHuagongshe Chemistry Print Report · For research reference only
N,N-Diethylaniline → 2-(4-tert-butylphenyl)-7-chloro-6-nitro-5H-[1,3,4]thiadiazolo[3,2-a]pyrimidin-5-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | N,N-Diethylaniline | HCID 7061 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | 2-(4-tert-butylphenyl)-7-hydroxy-6-nitro-5H-[1,3,4]thiadiazolo[3,2-a]pyrimidin-5-one | HCID 135802451 | — |
| Product | 2-(4-tert-butylphenyl)-7-chloro-6-nitro-5H-[1,3,4]thiadiazolo[3,2-a]pyrimidin-5-one | HCID 13591834 | — |
Reaction Steps
6.0 g of 2-(4-tert-butylphenyl)-7-hydroxy-6-nitro-5H-[1,3,4]thiadiazolo[3,2-a]pyrimidin-5-one was added to a mixture of 25 ml of phosphorus oxychloride and 4 ml of diethylaniline, and the resulting mixture was heated at a temperature of 70° to 80° C. for 2 hours. After cooling, the precipitate formed was filtered, washed successively with water, isopropanol and diethyl ether to obtain 4.3 g of 2-(4-tert-butylphenyl)-7-chloro-6-nitro-5H-[1,3,4]thiadiazolo[3,2-a]pyrimidin-5-one as crystals having a melting point of 245° to 248° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04652646 |
| Source dataset | uspto-grants-1987_03 |
| ORD ID | ord-3bee438ad1ee4bb59939b956547740ef |
| Source note | uspto-grants-1987_03 |