HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → TC-S 7001
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 2-Amino-4,6-dichloropyrimidine | HCID 65522 | — |
| Reactant | HCID 59740981 | HCID 59740981 | — |
| Solvent | Water | HCID 962 | — |
| Product | TC-S 7001 | HCID 11524200 | — |
Reaction Steps
415 mg (1.51 mmol) of 3,5-difluoro-4-[(3-methyl-1H-pyrrolo[2,3-b]pyridin-4-yl)oxy]aniline and 321 mg (1.96 mmol) of 4,6-dichloropyrimidine-2-amine are suspended in 8 ml of water. 1.96 ml of 1N hydrochloric acid are added, and the mixture is heated at reflux overnight. Using 1N aqueous sodium hydroxide solution, the pH is then adjusted to 10, resulting in the precipitation of crystals. The crystals are filtered off with suction and washed with water. The crude product is purified by column chromatography on silica gel (mobile phase: dichloromethane/methanol (7N ammonia) 100:1 to 100:5).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08329716B2 |
| Source dataset | uspto-grants-2012_12 |
| ORD ID | ord-63a6b94829fb48e986929c6b80431832 |
| Source note | uspto-grants-2012_12 |