HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 19045329, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 1′-Acetyl-6-nitrospiro[2H-indene-2,4′-piperidin]-1(3H)-one | HCID 19045538 | — |
| Catalyst | titanium(III) trichloride | HCID 10313229 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 19045329 | HCID 19045329 | 112.3% |
Reaction Steps
To a solution of 0.29 g (1.0 mmole) 1'-acetyl-1,3-dihydro-6-nitro-1-oxospiro[2H-indene-2,4'-piperidine] in 4 ml acetic acid was added 3.75 ml (4.3 mmoles) of 15% titanium (III) chloride solution in 20-30% aqueous hydrochloric acid dropwise and portionwise over 2 hours. The reaction mixture was made basic (pH 10) with saturated sodium bicarbonate solution and 10N sodium hydroxide solution, diluted with 50 ml water, and extracted with 3×50 ml ethyl acetate. The combined extracts were washed with 20 ml water and brine, dried, and the solvent was removed in vacuo to give 0.29 g crude 1'-acetyl-6-amino-1,3-dihydro-1-oxospiro[2H-indene-2,4'-piperidine].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05633247 |
| Source dataset | uspto-grants-1997_05 |
| ORD ID | ord-55054c5686e74d75b17896bf1ce5c7ef |
| Source note | uspto-grants-1997_05 |