HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 53909736, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 54456548 | HCID 54456548 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 53909736 | HCID 53909736 | 95.7% |
Reaction Steps
To a solution of 2,6-dimethyl-1-hydroxymethyl-3-[N-methyl-N-[4-(methylcarbamoyl) cinnamoylglycyl]amino]benzene (2.00 g) in N,N-dimethylformamide (100 ml) was added methanesulfonyl chloride (784 mg) under ice-cooling, and the mixture was stirred for 2 hours at the same temperature and overnight at ambient temperature. To the mixture was added water and extracted with chloroform. The organic layer was washed with brine, dried over magnesium sulfate and concentrated. The residue was pulverized with diethyl ether to give 1-chloromethyl-2,6-dimethyl-3-[N-[4-(methylcarbamoyl)cinnamoylglycyl]-N-methylamino]benzene (2.00 g) as white powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05994368 |
| Source dataset | uspto-grants-1999_11 |
| ORD ID | ord-2ba570968c1647309c8ec42cd9203a8f |
| Source note | uspto-grants-1999_11 |