Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Dichloromethane methanol | HCID 21226129 | — |
| Reactant | HCID 69214978 | HCID 69214978 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 18538868 | HCID 18538868 | 56.8% |
Reaction Steps
To a solution of the compound obtained in Example 233 (200 mg, 0.37 mmol) in ethanol (2 mL) was added aqueous solution of 1N-sodium hydroxide (0.56 mL, 0.56 mmol), and the mixture was stirred at 80° C. for 3 hours. To the mixture was added, dropwise aqueous solution of 1N-hydrochloric acid (0.56 mL, 0.56 mmol) under ice cooling, and the mixture was concentrated under reduced pressure. The concentrate was subjected to flash column chromatography (silica gel 20 g, dichloromethane/methanol=20/1 to 2/1), and the desired fraction was concentrated under reduced pressure. To the concentrate was added diisoprpyl ether, and the resulting precipitates were collected by filtration to give the titled compound (120 mg, 0.21 mmol, Yield 56%) as white amorphous substance.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US07348324B2 |
|---|
| Source dataset | uspto-grants-2008_03 |
|---|
| ORD ID | ord-82959ddce314495faa43766f5712a0e3 |
|---|
| Source note | uspto-grants-2008_03 |
|---|