HuagongsheHuagongshe Chemistry Print Report · For research reference only
N-Acetylsulfanilyl chloride → [(3aS,4R,6aR)-2,3,3a,4,5,6a-hexahydrofuro[2,3-b]furan-4-yl] N-[(1S,2R)-3-[(4-acetamidophenyl)sulfonyl-(4-cyano-2,2-dimethyl-butyl)amino]-1-benzyl-2-hydroxy-propyl]carbamate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | N-Acetylsulfanilyl chloride | HCID 8481 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | [(1S, 2R)-1-Benzyl-3-(4-cyano-2,2-dimethylbutylamino)-2-hydroxy-propyl]-carbamic acid (3R,3aS,6aR)hexahydro-furo[2,3-b]furan-3-yl ester | HCID 59815752 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | [(3aS,4R,6aR)-2,3,3a,4,5,6a-hexahydrofuro[2,3-b]furan-4-yl] N-[(1S,2R)-3-[(4-acetamidophenyl)sulfonyl-(4-cyano-2,2-dimethyl-butyl)amino]-1-benzyl-2-hydroxy-propyl]carbamate | HCID 480326 | 18.7% |
Reaction Steps
[(1S,2R)-1-Benzyl-3-(4-cyano-2,2-dimethyl-butylamino)-2-hydroxy-propyl]-carbamic acid (3R,3aS,6aR)hexahydro-furo[2,3-b]furan-3-yl ester (0.020 g, 0.05 mmol) was dissolved in CH2Cl2 and treated with diisopropylethylamine (0.016 ml, 0.09 mmol) and 4-acetamidobenzenesulfonyl chloride (0.011 g, 0.05 mmol) at ambient temperature under argon with stirring. After 15 h the reaction mixture was concentrated in vacuo, taken up in EtOAc, washed with sat. aq. NaHCO3, and brine. The organic phase was dried over MgSO4, filtered and solvent removed in vacuo. Purification by preparative thin layer chromatography (EtOAc) gave 0.006 g of a white solid. MS (ES): 643 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07919523B2 |
| Source dataset | uspto-grants-2011_04 |
| ORD ID | ord-a380e943ee5b4cd6883e723110f289ae |
| Source note | uspto-grants-2011_04 |