HuagongsheHuagongshe Chemistry Print Report · For research reference only
Carbamic acid, N-(4,6-dimethoxy-2-pyrimidinyl)-, phenyl ester → Amidosulfuron
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Carbamic acid, N-(4,6-dimethoxy-2-pyrimidinyl)-, phenyl ester | HCID 10945667 | — |
| Reactant | Methanesulfonamide, N-(aminosulfonyl)-N-methyl- | HCID 11084607 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | Amidosulfuron | HCID 91777 | 98.4% |
Reaction Steps
37.6 g of (N-methylsulfonyl-N-methylamino)sulfonamide are dissolved in 500 ml of acetonitrile, 55.0 g of phenyl 4,6-dimethoxy-2-pyrimidylcarbamate are added dropwise at room temperature, and the mixture is stirred for 18 hours at room temperature. Approx. 400 ml of acetonitrile are distilled off, and then 200 ml of water are added at 0° C., and the mixture is brought to pH 2-3 using 2N HCl. The product which has precipitated is filtered off with suction and washed with water. 72.6 g of the desired product of a purity of 98.4% are obtained, which corresponds to a yield of 96.8% of theory. The melting point of the product is 185-186° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05155222 |
| Source dataset | uspto-grants-1992_10 |
| ORD ID | ord-02e82f3055f041f892d599eb871cbcfc |
| Source note | uspto-grants-1992_10 |