HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 13362530, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 13556939 | HCID 13556939 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 13362530 | HCID 13362530 | — |
Reaction Steps
A solution of 3.7 g (9.7 mmole) of 9-chloro-7-(2-fluorophenyl)-5H-pyrimido[5,4-d][2]benzazepin-5-ol acetate in a mixture of 25 ml of tetrahydrofuran, 50 ml of methanol and 2 ml of 3N sodium hydroxide was stirred at room temperature for 0.5 hr. The reaction mixture was poured into ice water and extracted with methylene chloride. The organic layer was seperated, dried over anhydrous sodium sulfate and concentrated in vacuo to dryness. The residue crystallized from a mixture of methylene chloride and ether to give a crude product melting at 186°-188° C. Recrystallization from a mixture of ether and methylene chloride gave the product as cream colored prisms, mp 196°-198° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04547581 |
| Source dataset | uspto-grants-1985_10 |
| ORD ID | ord-99f424259cb84464ac26980ea69b4da8 |
| Source note | uspto-grants-1985_10 |