HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → 4-(tetrahydropyran-4-ylmethyl)-6-amino-3,4-dihydro-2H-1,4-benzoxazin-3-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 6-amino-3,4-dihydro-2H-1,4-benzoxazin-3-one | HCID 2763681 | — |
| Reactant | 4-(Bromomethyl)oxane | HCID 2773286 | — |
| Solvent | Water | HCID 962 | — |
| Product | 4-(tetrahydropyran-4-ylmethyl)-6-amino-3,4-dihydro-2H-1,4-benzoxazin-3-one | HCID 14441461 | 64% |
Reaction Steps
4.9 g (0.03 mol) of 6-amino-3,4-dihydro-2H-1,4-benzoxazin-3-one is introduced into 50 ml of dimethylformamide. At 5° C., 0.79 g (0.033 mol) of sodium hydride is added, and the mixture is stirred for 30 minutes at this temperature. Subsequently, 5.9 g (0.033 mol) of 4-bromomethyltetrahydropyran is added, the mixture is stirred for 3 hours at 60° C., 200 ml of water is added, extraction is carried out twice with methylene chloride, followed by drying and evaporation of the solvent under reduced pressure. There is obtained 5 g (64%) of 4-(tetrahydropyran-4-ylmethyl)-6-amino-3,4-dihydro-2H-1,4-benzoxazin-3-one as an oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05213605 |
| Source dataset | uspto-grants-1993_05 |
| ORD ID | ord-5fa8ee3feb184766b9f94cb19b21f45b |
| Source note | uspto-grants-1993_05 |