HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzene → HCID 19041763, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzene | HCID 241 | — |
| Reactant | 1,3-Propanediol | HCID 10442 | — |
| Reactant | Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) | HCID 466102 | — |
| Reactant | 3-Iodo-4,5-dimethoxybenzaldehyde | HCID 2778113 | — |
| Solvent | Benzene--water (1/1) | HCID 22272175 | — |
| Product | HCID 19041763 | HCID 19041763 | — |
Reaction Steps
3,4-dimethoxy-5-iodobenzaldehyde (41) (FIG. 22) (5.814 g,19.9 mmole), 1,3-propanediol (6.13 g, 79.6 mmole), pyridinium para-toluenesulfonate (2.0 g, 7.96 mmole) and 100 ml dry benzene were refluxed with Dean-Stark removal of the benzene-water azeotrope overnight. The benzene was removed in vacuo and the remaining oil redissolved in diethyl ether and was washed with 10% NaHCO3 and H2O. The organic layer was washed over MgSO4, and concentrated to a white solid in vacuo. (6.823 g, 98%). The solid can be recrystallized from hexane/ethyl acetate.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05639782 |
| Source dataset | uspto-grants-1997_06 |
| ORD ID | ord-cb837c098b784ba3ae9d4d17364d34f5 |
| Source note | uspto-grants-1997_06 |