Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 21498254 | HCID 21498254 | — |
| Product | HCID 21498295 | HCID 21498295 | — |
Reaction Steps
Phosphoryl chloride (1.68 g) was added dropwise to cooled dimethyl-formamide (1.60 g). A suspension of 1,5-dibenzyl-4,5,6,7-tetrahydro-7-methyl-2-phenyl-1H-pyrrolo[3,2-c]pyridine (3.92 g) in dimethylformamide (20 ml) was added portionwise. The resulting red solution was heated at 50° C for 4 hours, allowed to cool and poured on to 250 g ice. The mixture was basified with 2N sodium hydroxide, warmed gently for a few minutes, and the solid product collected by filtration, washed with water and dried. Two recrystallisations from methanol gave 2.86 g of the title compound as white needles. M.pt. 120°-1°. (Found: C, 83.2; H, 6.9; N, 6.5. C29H28N2O requires: C, 82.8; H, 6.7; N, 6.7%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US03992544 |
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| Source dataset | uspto-grants-1976_11 |
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| ORD ID | ord-5cca88676aed408cbf7af685dab0ee82 |
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| Source note | uspto-grants-1976_11 |
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