HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric Acid → 4-(Hydroxymethyl)-1-methylpyrrolidin-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | 1-Methyl-5-oxo-pyrrolidine-3-carboxylic acid methyl ester | HCID 108402 | — |
| Reactant | Lithium borohydride | HCID 4148881 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | 4-(Hydroxymethyl)-1-methylpyrrolidin-2-one | HCID 21914263 | — |
Reaction Steps
A solution of 2.3g (106 m moles) of LiBH4 in 150 ml of diethyl ether was slowly added dropwise at +5° C to 17.0g (107 m mols) of 4-carbomethoxy-1-methyl-pyrrolidone in 20 ml of absolute diethyl ether. Stirring was continued for 2 hours at room temperature, then the mixture was acidified with 2N sulfuric acid (pH 2), the solvent and water were distilled off to a large extent in vacuo and the remaining residue was extracted with methylene chloride. The dried methylene chloride phase was concentrated and the residue was distilled in vacuo. 5 g of the compounds desired were obtained in a 98 % purity: nD20 : 1.4950.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04071530 |
| Source dataset | uspto-grants-1978_01 |
| ORD ID | ord-4332e064dc1744829d6ee52788002db0 |
| Source note | uspto-grants-1978_01 |