Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 68642064 | HCID 68642064 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 68642063 | HCID 68642063 | 96% |
Reaction Steps
lithium aluminum hydride (0.21 g, 5.40 mmol) was suspended in tetrahydrofuran (15 ml), and under an ice cooling, a solution (5 ml) of ethyl 2-methyl-1,2,3,4-tetrahydrobenzo[4,5]imidazo[1,2-a]pyrazine-8-carboxylate (0.70 g, 2.70 mmol) prepared in the Step 38-1-6 in tetrahydrofuran was slowly added dropwise to the suspension. After the mixture was stirred for 30 minutes under an ice cooling, and a saturated sodium bicarbonate solution was slowly added to the mixture under an ice cooling. Ethyl acetate was slowly added to the resulting mixture, and the precipitate was removed by filtration. The residue separated by filtration was carefully washed with chloroform. The washings and the filtrate were concentrated together. The concentrate was purified by silica gel column chromatography (chloroform:methanol=10:1 to 5:1) to give the title compound (0.56 g, 96%) as a white powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US09200008B2 |
|---|
| Source dataset | uspto-grants-2015_12 |
|---|
| ORD ID | ord-5cda12a2bb7c4647b75167f3c4380366 |
|---|
| Source note | uspto-grants-2015_12 |
|---|