HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetonitrile → N-[8-chloro-5-(4-chlorophenyl)-5H-indeno[1,2-d]pyrimidin-5-yl]acetamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetonitrile | HCID 6342 | — |
| Reactant | Potassium Bicarbonate | HCID 516893 | — |
| Reactant | 8-chloro-5-(4-chlorophenyl)-5H-indeno[1,2-d]pyrimidin-5-ol | HCID 14257087 | — |
| Solvent | Methanesulfonic Acid | HCID 6395 | — |
| Product | N-[8-chloro-5-(4-chlorophenyl)-5H-indeno[1,2-d]pyrimidin-5-yl]acetamide | HCID 14257092 | — |
Reaction Steps
A mixture of 3.0 g of 8-chloro-5-(4-chlorophenyl)-5H-indeno[1,2-d]pyrimidin-5-ol in 15 ml of acetonitrile and 50 ml of methanesulfonic acid were stirred for approximately 18 hours. The reaction mixture was added to a large excess of a potassium bicarbonate solution and the resulting mixture was extracted with ethyl acetate. The organic layer was washed with a saturated sodium chloride solution, dried over magnesium sulfate, and concentrated in vacuo. Crystallization from acetonitrile/water provided 2.53 g of the desired title product, m.p. 238°-241° C. Two further recrystallizations provided material with a melting point of 245°-248° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04769378 |
| Source dataset | uspto-grants-1988_09 |
| ORD ID | ord-9e73b667e8c84cd48ce28747039a3937 |
| Source note | uspto-grants-1988_09 |