HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl N-(triethylammoniosulfonyl)carbamate → HCID 68000904, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl N-(triethylammoniosulfonyl)carbamate | HCID 2724994 | — |
| Reactant | HCID 68000416 | HCID 68000416 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | 1,1-Dichloroethane | HCID 6365 | — |
| Product | HCID 68000904 | HCID 68000904 | — |
Reaction Steps
A solution of 58 mg (0.115 mmol) of (S)-N′-acetyl-2-((3S,5R,6S)-3-allyl-5-(3-chlorophenyl)-6-(4-chlorophenyl)-2-oxopiperidin-1-yl)butanehydrazide (Example 34, Step A) and Burgess' reagent (110 mg, 0.462 mmol) in dichloroethane (1154 μL) was heated in the microwave at 120° C. for 30 min. Then the reaction mixture was diluted with water and extracted with DCM. The combined organic layers were washed with sat. aq. NaCl and NaHCO3-solutions, dried over Na2SO4, filtered and the filtrate was concentrated under reduced pressure. Separation by reversed phase HPLC (55 to 90% MeCN/H2O in 35 min, 29 mg injection each time) provided the title compound as a colorless film. MS (ESI) 484.1 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09296736B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-2bf45969b4db4cb2bc24728c67b98194 |
| Source note | uspto-grants-2016_03 |