HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,3-Dihydroxybutanedioic Acid → 4-[(5,6,7,8-Tetrahydro-5,5,8,8-tetramethylnaphth-2-yl)ethynyl]-benzaldehyde
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,3-Dihydroxybutanedioic Acid | HCID 875 | — |
| Reactant | 4-[(5,6,7,8-Tetrahydro-5,5,8,8-tetramethylnaphth-2-yl)ethynyl]-benzonitrile | HCID 13604826 | — |
| Reactant | Diisobutylaluminumhydride | HCID 21225700 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Hexane | HCID 8058 | — |
| Product | 4-[(5,6,7,8-Tetrahydro-5,5,8,8-tetramethylnaphth-2-yl)ethynyl]-benzaldehyde | HCID 19786963 | 38% |
Reaction Steps
56 ml (67 millimoles) of a 20% strength solution of diisobutylaluminum hydride in hexane were added to a solution of 10 g (32 millimoles) of 4-[(5,6,7,8-tetrahydro-5,5,8,8-tetramethylnaphth-2-yl)-ethynyl]-benzonitrile (Example 1) in 120 ml of absolute ether. The mixture was stirred for a further 40 minutes, 150 ml of saturated tartaric acid solution were added dropwise and stirring was continued for a further hour. Thereafter, the mixture was extracted three times with ether and the combined ether phases were washed twice with water, dried over Na2SO4 and evaporated down. Recrystallization of the residue from isopropanol gave 3.8 g (38%) of the title compound of melting point 130° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05126371 |
| Source dataset | uspto-grants-1992_06 |
| ORD ID | ord-90df314daa8241358ded0f25f8fc79ac |
| Source note | uspto-grants-1992_06 |