Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethylene Glycol | HCID 174 | — |
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | HCID 13152886 | HCID 13152886 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 54566081 | HCID 54566081 | — |
Reaction Steps
A mixture of 5 gm. of 6,11-dihydro-2-formyl-5H-pyrrolo[2,1-b][3]benzazepin-11-one, 2.5 gm. of ethylene glycol, 0.5 gm. of p-toluenesulfonic acid and 100 ml. of toluene is refluxed for 16 hr. in an apparatus designed to remove water formed during the reaction (Dean-Stark apparatus). The reaction mixture is cooled to 0° C. and washed rapidly with ice cold 5% sodium carbonate solution (2 × 50 ml.) and dried over Na2SO4. Evaporation of the solvent leaves 6,11-dihydro-2-(2-dioxolanyl)-5H-pyrrolo[2,1-b][3]benzazepin-11-one as an oil which is of sufficient purity for use in the next step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04112112 |
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| Source dataset | uspto-grants-1978_09 |
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| ORD ID | ord-9c0a6172a7434d588f2784a043e52290 |
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| Source note | uspto-grants-1978_09 |
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