Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Isopropanol | HCID 3776 | — |
| Reactant | 2-(Methylamino)ethanol | HCID 8016 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | Benzoyl chloride, 2-chloro-5-nitro- | HCID 117637 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 14574097 | HCID 14574097 | — |
| Product | HCID 14574098 | HCID 14574098 | — |
Reaction Steps
260 g of N-(2-hydroxyethyl)-N-methyl-2-chloro-5-nitrobenzamide, which is prepared from 2-chloro-5-nitrobenzoyl chloride and 2-(methylamino)-ethanol, are heated to reflux temperature in 500 ml of water/500 ml of isopropanol. A solution of 65 g of potassium hydroxide in 250 ml of water is added dropwise in the course of one hour and the mixture is maintained at reflux temperature for a further 3 hours. The pH is lowered to 9, the reaction solution is cooled to 0° C. and the crystalline precipitate is filtered off with suction and dried. 174 g of 7-nitro-4-methyl-2,3-dihydro-1,4-benzoxazepin-5-one of melting point 116° C. are obtained. ##STR21##
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05041629 |
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| Source dataset | uspto-grants-1991_08 |
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| ORD ID | ord-028f0350c365445cb5fa8056e7b05ce2 |
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| Source note | uspto-grants-1991_08 |
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