HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 68685438, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 1-Propanol, 3-amino-2,2-dimethyl- | HCID 117326 | — |
| Reactant | 5-((4-Chlorobenzamido)methyl)thiophene-2-sulfonyl chloride | HCID 2735713 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 68685438 | HCID 68685438 | — |
Reaction Steps
To a stirred solution of 2 equivalents of 3-Amino-2,2-dimethyl-propan-1-ol (1.0 g, 10 mmol) in DMF in the presence of 2 equivalents of DIEA (1.7 ml, 10 mMol) is added a solution of sulfonylchloride (1b) (1.75 g, 5 mMol, 1 equivalent) in DMF. The reaction mixture is stirred for 12 h at room temperature. DCM is added and any excess of amine is extracted into 0.1N HCl solution. The organic phase is washed with brine and dried over MgSO4. 4-Chloro-N-[5-(3-hydroxy-2,2-dimethyl-propylsulfamoyl)-thiophen-2-ylmethyl]-benzamide (compound of formula XII) is obtained after evaporation of the solvent. LC-MS analysis and NMR analysis showed that the compound was pure enough to carry on the next step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07683078B2 |
| Source dataset | uspto-grants-2010_03 |
| ORD ID | ord-04829a1866234c81b1666141bcc680bf |
| Source note | uspto-grants-2010_03 |