HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 90403561, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 90403134 | HCID 90403134 | — |
| Product | HCID 90403561 | HCID 90403561 | 72.4% |
Reaction Steps
A solution of N-tert-butyl-1-(7-(4-chlorobenzyl)-3-methyl-2,6-dioxo-8-(3-(trifluoromethoxy)phenoxy)-2,3,6,7-tetrahydro-1H-purin-1-yl)methanesulfonamide (120 mg, 0.195 mmol, example 71) in TFA (2 ml, 26.9 mmol) was stirred at 50° C. for 16 h. The mixture was concentrated and then purified by silica gel chromatography eluting with DCM/methanol (40:1) to give (7-(4-chlorobenzyl)-3-methyl-2,6-dioxo-8-(3-(trifluoromethoxy)phenoxy)-2,3,6,7-tetrahydro-1H-purin-1-yl)methanesulfonamide (79 mg, 72.4% yield) as white solid. 1H-NMR (DMSO-d6) δ 7.65-7.61(t, 1H), 7.49(s, 1H), 7.47-7.41(m, 6H), 7.36-7.35(d, 1H), 7.05(s, 2H), 5.45(s, 2H), 5.23(s, 2H), 3.31(s, 3H). LCMS retention time 3.004 min; LCMS MH+ 560.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09359359B2 |
| Source dataset | uspto-grants-2016_06 |
| ORD ID | ord-c6ec551589e44d49b33d51d3bf0f2814 |
| Source note | uspto-grants-2016_06 |