HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Methylpiperazine → 2-Methoxycarbonyl-3-chloro-4-((4-methylpiperazin-1-yl)methyl)thiophene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Methylpiperazine | HCID 53167 | — |
| Reactant | Methyl 4-(bromomethyl)-3-chlorothiophene-2-carboxylate | HCID 18376575 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 2-Methoxycarbonyl-3-chloro-4-((4-methylpiperazin-1-yl)methyl)thiophene | HCID 18376752 | 40% |
Reaction Steps
To 2-methoxycarbonyl-3-chloro-4-(bromomethyl)thiophene (0.20 g, 0.74 mmol) in methylene chloride (7.5 mL) was added 1-methylpiperazine (0.095 mL, 0.86 mmol) and the mixture was stirred at ambient temperature. After 16 hours, the mixture was poured onto methylene chloride (20 mL) and washed with dilute aqueous NaHCO3, water and brine, dried over Na2SO4 and concentrated in vacuo. Purification by flash chromatography on silica gel afforded 0.085 g (40% yield) of 2-methoxycarbonyl-3-chloro-4-((4-methylpiperazin-1-yl)methyl)thiophene as a tan solid; NMR (CDCl3) 7.4 (s, 1), 3.9 (s, 3), 3.5 (s, 2), 2.3-2.7 (br m, 8), 2.2 (s, 3) ppm.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06380221B1 |
| Source dataset | uspto-grants-2002_04 |
| ORD ID | ord-55125023bcf44ac08491b2234f506c63 |
| Source note | uspto-grants-2002_04 |