HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → tert-butyl 5-(N-methyl-2-nitrophenylsulfonamido)pentylcarbamate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Tert-butyl 5-(2-nitrophenylsulfonamido)pentylcarbamate | HCID 67226448 | — |
| Solvent | Acetone | HCID 180 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Diisopropyl Ether | HCID 7914 | — |
| Product | tert-butyl 5-(N-methyl-2-nitrophenylsulfonamido)pentylcarbamate | HCID 86652975 | 93.7% |
Reaction Steps
To a mixture of tert-butyl 5-(2-nitrophenylsulfonamido)pentylcarbamate 30c (32.61 g, 84 mmoles) and potassium carbonate (13.96 g, 1.2 eq) in acetone (300 mL) was added methyl iodide (5.5 mL, 1.05 eq). After stirring at RT overnight, more methyl iodide (1 eq) and potassium carbonate (0.6 eq) was added and the RM was stirred at RT until completion. The RM was then diluted with water and extracted with DCM. The organic layer was separated, washed with brine, dried over magnesium sulfate, filtered and concentrated. Trituration in diisopropyl ether afforded 31.59 g (93% yield) of tert-butyl 5-(N-methyl-2-nitrophenylsulfonamido)pentylcarbamate 30d as a white solid; m/z 402 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09427440B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-a8aff868c05348d098e8a376cf009d53 |
| Source note | uspto-grants-2016_08 |