HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,3-Dichloroacetone → 4-(Chloromethyl)-2-(propan-2-yl)-1,3-thiazole--hydrogen chloride (1/1)
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,3-Dichloroacetone | HCID 10793 | — |
| Reactant | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| Reactant | 2-Methylpropanethioamide | HCID 10909507 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | 4-(Chloromethyl)-2-(propan-2-yl)-1,3-thiazole--hydrogen chloride (1/1) | HCID 18758846 | — |
Reaction Steps
A mixture of 94.0 g (0.91 mol) of 2-methylpropane-thioamide, 115.7 g (0.91 mol) of 1,3-dichloroacetone, and 109.7 g (0.91 mol) of MgSO4 in 1.6 liters of acetone was heated at reflux for 3.5 h. The resulting mixture was allowed to cool, filtered, and the solvent was removed in vacuo to provide the crude desired compound as a yellow oil. 1H NMR (DMSO-d6) δ1.32 (d, J=7 Hz, 6H), 3.27 (heptet, J=7 Hz, 1H), 4.78 (s, 2H), 7.61 (s, 1H). Mass spectrum: (M+H)+ =176.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05696270 |
| Source dataset | uspto-grants-1997_12 |
| ORD ID | ord-fe2be305820e46478999bd5e3639fc4c |
| Source note | uspto-grants-1997_12 |