HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 11961256, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | N,N-Dimethyl-1,3-propanediamine | HCID 7993 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 5-[2-(Acetylamino)-4-methyl-1,3-thiazol-5-yl]thiophene-2-sulfonyl chloride | HCID 86622562 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 11961256 | HCID 11961256 | — |
Reaction Steps
5-[2-(acetylamino)-4-methyl-1,3-thiazol-5-yl]thiophene-2-sulfonyl chloride, prepared as in Step II of Example 1 (280 mg; 0.84 mmol; 1 eq), is dissolved in DCM (10 ml). N,N-dimethylpropane-1,3-diamine (0.89 ml; 8.4 mmol; 10 eq) and DIEA (0.17 ml; 0.98 mmol; 3 eq) are added. After one night reaction, water (1 ml) is added and the solvents are evaporated to dryness. The crude product is re-dissolved in DCM and washed with NH4Cl saturated solution, water and dried over MgSO4. After evaporation of the solvents, crude material is precipitated in a mixture of DCM and diethyl ether, affording after filtration, Compound (10) as a white solid (105 mg; 28%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08399497B2 |
| Source dataset | uspto-grants-2013_03 |
| ORD ID | ord-b41937d757764d7b8b742ad47210ef62 |
| Source note | uspto-grants-2013_03 |