HuagongsheHuagongshe Chemistry Print Report · For research reference only
Stannous chloride dihydrate → Dimethylcarbamic acid 3-(3-amino-2-fluorobenzyl)-4-fluoromethyl-2-oxo-2H-1-benzopyran-7-yl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Stannous chloride dihydrate | HCID 61436 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 59139149 | HCID 59139149 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | Dimethylcarbamic acid 3-(3-amino-2-fluorobenzyl)-4-fluoromethyl-2-oxo-2H-1-benzopyran-7-yl ester | HCID 59139194 | 102.5% |
Reaction Steps
Ethyl acetate (2.0 mL) was added to dimethylcarbamic acid 4-fluoromethyl-3-(2-fluoro-3-nitrobenzyl)-2-oxo-2H-1-benzopyran-7-yl ester (20.5 mg) (6c-1-4), and tin(II) chloride dihydrate (60 mg) was added to the resultant suspension while stirring at room temperature. The suspension was heated under reflux for 1.5 hours, and after cooling to room temperature, saturated sodium hydrogen carbonate was added, and the mixture was extracted with ethyl acetate. The resultant organic layer extraction liquid was washed with saturated saline, and the organic layer was dried over anhydrous magnesium sulfate. The solvent was then distilled away under reduced pressure to yield the title compound (19.5 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08569378B2 |
| Source dataset | uspto-grants-2013_10 |
| ORD ID | ord-5aa153d08a044fb09b87cca4b1d0ea92 |
| Source note | uspto-grants-2013_10 |