HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tert-Butyl nitrite → HCID 18446121, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tert-Butyl nitrite | HCID 10906 | — |
| Reactant | Dimethyl Disulfide | HCID 12232 | — |
| Reactant | 4-Bromo-3-methyl-2-methylsulfonylaniline | HCID 18446120 | — |
| Catalyst | Copper | HCID 23978 | — |
| Product | HCID 18446121 | HCID 18446121 | — |
Reaction Steps
75 g of copper powder and 100 ml of dimethyl disulfide were added to 92 g (0.8 mol) of tert-butyl nitrite. At 50–52° C., a solution of 142 g (0.54 mol) of 4-bromo-3-methyl-2-methylsulfonyl aniline in 600 ml of dimethyl disulfide was added dropwise, and the mixture was stirred at 50–55° C. for 7 hours. After cooling, the mixture was filtered off with suction through kieselguhr, and dichloromethane was added to the filtrate. The organic phase was washed with dilute hydrochloric acid and then with water. After drying over sodium sulfate, the organic phase was concentrated under high vacuum. This gave 170 g of the title compound as a black oil which was used for the next reaction step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07196229B2 |
| Source dataset | uspto-grants-2007_03 |
| ORD ID | ord-a881e726e1a6408c8e022af07c53ad6d |
| Source note | uspto-grants-2007_03 |