HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 178484030, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Sodium cyanoborohydride | HCID 5003444 | — |
| Reactant | HCID 178478680 | HCID 178478680 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 178484030 | HCID 178484030 | — |
Reaction Steps
To a solution of 0.685 g of the compound of Example 1 (1.95 mmol) in 18 ml of methanol there are added, at 0° C., 0.245 g of sodium cyanoborohydride, 0.56 ml of acetic acid and then, dropwise, 0.4 ml of 37% formaldehyde solution in water. After stirring for 4 hours, 2 ml of saturated aqueous potassium carbonate solution are added. After evaporating off the solvents and then diluting with water, the mixture is extracted with ethyl acetate, dried (MgSO4) and evaporated. The residue obtained is purified by chromatography on a silica column using a mixture of dichloromethane/methanol/ammonium hydroxide (80/20/2) as eluant to yield, after converting to a salt in ethanol in the warm state using 1N ethereal HCl, the title product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08247441B2 |
| Source dataset | uspto-grants-2012_08 |
| ORD ID | ord-66715978740f4d8e8334a5d573f87747 |
| Source note | uspto-grants-2012_08 |