Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | HCID 18180077 | HCID 18180077 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 18180093 | HCID 18180093 | 111.9% |
Reaction Steps
A mixture of 1-(6-methoxy-2-methyl-3-nitrophenyl)-4-methylpiperazine (D30) (360 mg, 1.36 mmol), dry dimethylsulfoxide (3 ml), paraformaldehyde (82 mg, 2.72 mmol) and potassium tert-butoxide (52 mg, 0.46 mmol) was heated at 70-75° C. for 30 h. After cooling, the mixture was partitioned between water and ethyl acetate. The organic phase was dried (Na2SO4) evaporated under reduced pressure and purified by chromatography on silica gel, eluting with methanol and dichloromethane, to give the title compound (D31) as a yellow solid (152 mg, 38%) MH+=296.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06423717B1 |
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| Source dataset | uspto-grants-2002_07 |
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| ORD ID | ord-3970f33bf66942f7be9ae3bac6eb2501 |
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| Source note | uspto-grants-2002_07 |
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