HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Butanol → 4-(5,5-Dimethyl-2-phenyl-1,3-dioxan-2-yl)-2-nitrobenzenamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Butanol | HCID 263 | — |
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | Neopentyl glycol | HCID 31344 | — |
| Reactant | 4-Amino-3-nitrobenzophenone | HCID 596970 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 4-(5,5-Dimethyl-2-phenyl-1,3-dioxan-2-yl)-2-nitrobenzenamine | HCID 21427096 | 55% |
Reaction Steps
A mixture of 31.5 parts of (4-amino-3-nitrophenyl)phenylmethanone, 21 parts of 2,2-dimethyl-1,3-propanediol, 2 parts of 4-methylbenzenesulfonic acid, 40 parts of butanol and 450 parts of methylbenzene is stirred and refluxed for 16 hours with water-separator. The reaction mixture is cooled and washed with ammonium hydroxide. The organic phase is dried, filtered and evaporated. The residue is crystallized from 2,2'-oxybispropane, yielding 27.5 parts (55%) of 4-(5,5-dimethyl-2-phenyl-1,3-dioxan-2-yl)-2-nitrobenzenamine; mp. 139.8° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04032536 |
| Source dataset | uspto-grants-1977_06 |
| ORD ID | ord-c54708484dbc44dbad4de6294514ee63 |
| Source note | uspto-grants-1977_06 |