HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 3,4-dihydro-4-methyl-7-(trifluoromethyl)-2H-1,4-benzodiazepine-2,5(1H)-dione
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sarcosine | HCID 1088 | — |
| Reactant | 6-(trifluoromethyl)-2,4-dihydro-1H-3,1-benzoxazine-2,4-dione | HCID 53867034 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | 3,4-dihydro-4-methyl-7-(trifluoromethyl)-2H-1,4-benzodiazepine-2,5(1H)-dione | HCID 21291979 | — |
Reaction Conditions
| Temperature | 110 °C |
|---|
Reaction Steps
A suspension of 5.76 g (24.9 mmole) of 5-(trifluoromethyl)isatoic acid anhydride and 2.44 g (27.4 mmol) of sarcosine in 8 ml of dimethyl sulphoxide is stirred at 110° C. for 4 hours, subsequently poured into 70 ml of water and evaporated to dryness in vacuo. After column chromatography on silica gel using ethyl acetate/n-hexane (9:1) for the elution and recrystallisation of the product from ethanol, there is obtained 3,4-dihydro-4-methyl-7-(trifluoromethyl)-2H-1,4-benzodiazepine-2,5(1H)-dione of melting point 203°-206° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04359420 |
| Source dataset | uspto-grants-1982_11 |
| ORD ID | ord-6bfbf21b4f044f159e09c4cb6091e9b2 |
| Source note | uspto-grants-1982_11 |