HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 68859059, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 68857906 | HCID 68857906 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 68859059 | HCID 68859059 | 64% |
Reaction Steps
(2-{5-Methyl-2-[3-(4-methylpiperazin-1-yl)-propylamino]-pyrimidin-4-yl}-benzo[b]thiophen-6-yl)-carbamic acid tert-butyl ester (0.33 g, 0.66 mmol) is dissolved in dichloromethane (6 mL) and TFA (0.78 mL) is added. The solution is stirred for 20 hours before adding methanol. The mixture is passed through an SCX column. After eluting with methanol, 20% of 2.0 M NH3/MeOH in EtOAc is used to elute the product which is then chromatographed on silica gel, eluting with 2.0 M NH3/MeOH in dichloromethane 0-15%, to give the title compound as a yellow oil. (166 mg, 64% yield). ES+(m/z) 397 [M+H].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07547691B2 |
| Source dataset | uspto-grants-2009_06 |
| ORD ID | ord-dd18d464272b4cb6b6209bdc8305d0bd |
| Source note | uspto-grants-2009_06 |