HuagongsheHuagongshe Chemistry Print Report · For research reference only
Aluminium lithium hydride → HCID 86732439, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 71553532 | HCID 71553532 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86732439 | HCID 86732439 | — |
Reaction Steps
80 mg of methyl 2,4-dichloro-3-({3-[5-methoxy-4-(pyridin-4-ylamino)pyrimidin-2-yl]-1H-indazol-1-yl}methyl)benzoate (2-16-1, 0.149 mmol, 1. eq.) was suspended in 2.4 ml of dry tetrahydrofuran under nitrogen atmosphere. The suspension was cooled with an ice bath to +3° C., upon which 254 μl of a 1 M lithium aluminium hydride solution in tetrahydrofuran (0.254 mmol, 1.7 eq.) were added dropwise. The ice bath was remove and the mixture was stirred at room temperature for 30 minutes. Then the mixture was acidified by 2 M sulfuric acid. The mixture formed a suspension which was filtered off and washed with water. The precipitate was dried in vacuo at 60° C. for 18 hours to yield 60 mg (0.11 mmol, 74.4%) of the analytically pure target compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09265763B2 |
| Source dataset | uspto-grants-2016_02 |
| ORD ID | ord-2d55f05624854e2ca6671b227c0e0165 |
| Source note | uspto-grants-2016_02 |