HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Nitropropane → 2-Bromo-4-methyl4-nitropentanal
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Nitropropane | HCID 398 | — |
| Reactant | Acrolein | HCID 7847 | — |
| Reactant | Bromine | HCID 24408 | — |
| Reactant | 4-Methyl-4-nitrovaleraldehyde | HCID 12264009 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Water | HCID 962 | — |
| Product | 4-Methyl-4-nitrovaleraldehyde | HCID 12264009 | — |
| Product | 2-Bromo-4-methyl4-nitropentanal | HCID 22038558 | 163.1% |
Reaction Steps
4-Methyl-4-nitropentanal is prepared by condensation of acrolein and 2-nitropropane according to a known procedure (Synthesis 1986, 237). To a solution of 4-methyl-4-nitropentanal (8.5 g, 58.56 mmol) in acetic acid (125 ml) is added bromine (9.12 g, 57.07 mmol) dropwise while the temperature is kept below 15° C. After stirring for 15 minutes at room temperature the reaction is poured into a mixture of water and ice (250 ml) and extracted two times with dichloromethane. The combined organic extracts are washed with water and with brine, successively, dried over magnesium sulfate, and the solvent is removed under reduced pressure to leave 10.7 g of 2-bromo-4-methyl-4-nitropentanal which is used for the next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07241772B2 |
| Source dataset | uspto-grants-2007_07 |
| ORD ID | ord-ee4863a0fae0447798e1eb7f2f458047 |
| Source note | uspto-grants-2007_07 |