HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Methylpiperazine → 5-{4-[(4-Methylpiperazin-1-yl)methyl]benzamido}-2-(naphthalen-2-ylamino)thiazole-4-carboxamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Methylpiperazine | HCID 53167 | — |
| Reactant | 4-(Chloromethyl)benzoyl chloride | HCID 70136 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 5-Amino-2-(naphthalen-2-ylamino)thiazole-4-carboxamide | HCID 86703369 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | Dimethylacetamide | HCID 31374 | — |
| Product | 5-{4-[(4-Methylpiperazin-1-yl)methyl]benzamido}-2-(naphthalen-2-ylamino)thiazole-4-carboxamide | HCID 72550854 | 11% |
Reaction Steps
To a mixture of 5-amino-2-(naphthalen-2-ylamino)thiazole-4-carboxamide (0.50 g, 1.76 mmol) and. N,N-diisopropylethylamine (0.3 mL, 1.94 mmol) in DMA (30 mL) was added 4-chloromethylbenzoyl chloride (0.37g, 1.94 mmol) at 0° C. The mixture was stirred for 3 hrs at rt. Then 1-methylpiperazine (0.1 mL, 0.95 mmol) was added to the mixture (0.083 g in 5 mL DMA), and the mixture was stirred for 16 hrs at rt. The reaction mixture was diluted with ethyl acetate (150 mL), washed with water, and dried over Na2SO4. The solvent was evaporated under reduced pressure, and the crude residue was purified by silica gel column chromatograph eluted with 5% MeOH in DCM to give 0.010 g (11% yield) of the titled compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09102637B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-954b9c94b4784ce980d33420695ee65d |
| Source note | uspto-grants-2015_08 |