HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric Acid → HCID 71611596, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 71611319 | HCID 71611319 | — |
| Product | HCID 71611596 | HCID 71611596 | — |
Reaction Steps
To 126 mg of 4-({2-[1-(2-fluorobenzyl)-5-methoxy-1H-pyrazol-3-yl]-5-methoxypyrimidin-4-yl}amino)pyridine-3-carbonitrile 2-1-7 (0.294 mmol, 1.0 eq.) were given at rt with caution 0.446 mL of sulfuric acid. The mixture was stirred for 24 hours at rt. Then the reaction mixture was dropped into ice water and set with aqueous 2 M sodium hydroxide solution to an alkaline pH. This aqueous layer was extracted three times with DCM/propan-2-ol 4:1. The combined organic layers were dried over magnesium sulfate and concentrated in vacuo. The crystallization from methanol provided 37.0 mg (0.08 mmol, 28%) of analytically pure target compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09422268B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-225e23c747034886946ac5edf332a394 |
| Source note | uspto-grants-2016_08 |