Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methane | HCID 297 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | HCID 14390493 | HCID 14390493 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Product | HCID 14390463 | HCID 14390463 | 11% |
Reaction Steps
Solid N-[3-[(2-methoxybenzoyl)amino]-2-pyridinyl]glycine ethyl ester, 13.75 g (0.042 mole) was heated in glass in a Wood's metal bath at 210°-20° C. for 2 minutes, then at 215°-20° C. for 2 minutes. The residue was dissolved in methylene chloride, treated with activated charcoal, and filtered through a Celite pad. The filtrate (dark orange) was treated with Florisil® to give a dark filtrate, which was evaporated to give an oil. The oil was dissolved in isopropyl alcohol, filtered and the filtrate acidified with methanolic hydrogen chloride and diluted with isopropyl ether. The crystalline crop was collected, washed with isopropyl ether-isopropyl alcohol (minimum), and dried under high vacuum at room temperature overnight to give 1.6 g (11%) of title compound, mp 177°-80° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04772600 |
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| Source dataset | uspto-grants-1988_09 |
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| ORD ID | ord-9eecc37db1294a44bce22a0f28217210 |
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| Source note | uspto-grants-1988_09 |
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