Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 1-Piperazinecarboxaldehyde | HCID 82191 | — |
| Reactant | Propanoyl chloride, 3-bromo- | HCID 84944 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 19884010 | HCID 19884010 | 70.7% |
Reaction Steps
A mixture of 15 ml of water and 25 ml of methylene chloride containing 3.0 g (36 mmole) of sodium bicarbonate and 2.82 g (24.7 mmole) of 1-piperazinecarboxaldehyde is stirred and treated with 5.0 g (30.9 mmole) of 3-bromopropionyl chloride in 10 ml of methylene chloride over a 15 minute period while maintaining a temperature of about 20° C. After stirring for an additional 20 minutes, the organic phase is separated and the aqueous phase is extracted with methylene chloride. The combined organic phases are drive (Na2SO4), filtered and concentrated under high vacuum to yield 4.35 g (70.2%) of product as a colorless solid: mp 96°-98° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US05015741 |
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| Source dataset | uspto-grants-1991_05 |
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| ORD ID | ord-9e561c3d251d451281b72c706db81564 |
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| Source note | uspto-grants-1991_05 |
|---|
