HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 69240704, compound → HCID 69241132, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 69240704 | HCID 69240704 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Product | HCID 69241132 | HCID 69241132 | 88.9% |
Reaction Steps
To a solution of 9.37 g of tert-butyl (1R,2S)-2-({2-[(4-methoxybenzyl)amino]-6-methylquinazolin-4-yl}amino)cyclohexylcarbamate in 30 ml of methylene chloride, 95 ml of trifluoroacetic acid was added under ice cooling, and then the mixture was stirred for 72 hours. The reaction solution was concentrated, neutralized with a saturated sodium hydrogencarbonate solution, extracted with chloroform:methanol=10:1 and then dried. The solvent was distilled off and the residue was purified by Fuji Silysia NH silica gel column chromatography (chloroform:methanol=50:1) to obtain 4.60 g of the desirable compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07718663B2 |
| Source dataset | uspto-grants-2010_05 |
| ORD ID | ord-c457cd6f1c0948ddb9843e388257c8ab |
| Source note | uspto-grants-2010_05 |