HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 18381603, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 18381655 | HCID 18381655 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 18381603 | HCID 18381603 | 61% |
Reaction Steps
In a Claisen flask, a suspension under N2 of 4-[4-(3,5-dichloro-pyridin-4-ylmethyl)-7-methoxy-phthalazin-1-yl]-2-methyl-but-3-yn-2-ol (0.4 g, 1 mmole), prepared as described in example 107, in dry toluene (50 ml) was added with a catalytic amount of NaH, the mixture was refluxed, then distilled up to half volume. The mixture was left to stand overnight, then poured into water, extracted three times with CH2Cl2, discoloured with charcoal, filtered over celite and dried to give a solid which was triturated in ethyl ether to give 0.21 g of the title compound. m.p.: 210.3-211.3° C. (dec.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06492360B1 |
| Source dataset | uspto-grants-2002_12 |
| ORD ID | ord-6e0996b390704733a9dbf7470f6604a3 |
| Source note | uspto-grants-2002_12 |