HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl morpholine oxide → HCID 11181123, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl morpholine oxide | HCID 82029 | — |
| Reactant | 6-(4-bromo-2-methyl-phenylamino)-7-fluoro-3-(4-thiomorpholin-4-yl-butyl)-3H-benzoimidazole-5-carboxylic acid cyclopropylmethoxy-amide | HCID 11273335 | — |
| Reactant | Methanol water acetone | HCID 86590524 | — |
| Catalyst | Osmium Tetroxide | HCID 30318 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | Sodium Thiosulfate | HCID 24477 | — |
| Product | HCID 11181123 | HCID 11181123 | 71% |
Reaction Steps
To a solution of 6-(4-bromo-2-methyl-phenylamino)-7-fluoro-3-(4-thiomorpholin-4-yl-butyl)-3H-benzoimidazole-5-carboxylic acid cyclopropylmethoxy-amide 181 (8 mg, 0.014 mmol) in 1:1:1 water/acetone/MeOH (1 mL) is added NMO (1.6 mg, 0.014 mmol) and osmium tetroxide (250 μL, 0.054 M solution in t-BuOH, 0.014 mmol). After stirring for 24 hours, the solution is diluted with saturated sodium thiosulfate, stirred for 10 minutes and diluted with ethyl acetate. The solution is washed with brine (2×), dried (Na2SO4) and concentrated under reduced pressure to a grey solid. FCC (10:1 dichloromethane/methanol) provides 6 mg (71%) desired product as an off-white solid. MS ESI (+) m/z 622, 624 (M+, Br pattern) detected.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07425637B2 |
| Source dataset | uspto-grants-2008_09 |
| ORD ID | ord-038ade63a58e4a4a953703c9ec2daa8b |
| Source note | uspto-grants-2008_09 |