Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Oxalic Acid | HCID 971 | — |
| Reactant | 2-(2-Methoxyphenoxy)ethyl amine | HCID 1713005 | — |
| Reactant | 4-Oxiranylmethoxy-9H-carbazole | HCID 5020710 | — |
| Solvent | Chlorobenzene | HCID 7964 | — |
| Product | HCID 24991929 | HCID 24991929 | — |
Reaction Steps
146.4 g (0.875 moles, 2.1 mol equivalents) of 2-(2-methoxy phenoxy)ethylamine is dissolved in 500 ml of monochlorobenzene and the temperature is raised 125° C. under stirring. 100 g (0.42 moles) of 4-(2,3-epoxy propoxy)carbazole is slowly added in lots over 1 hr at reflux temperature. Reflux is then carried on for two hrs. Distilled of the monochlorobenzene under vacuum followed by cooling of the reaction mass to 50-60° C. 1000 ml isopropyl acetate is charged followed by the addition of 1000 ml DM water. pH of reaction mass is adjusted to 2.0-2.5 with 10% oxalic acid solution at 45° C.-50° C. Stirred for one hr at 45° C.-50° C., the reaction mass is cooled to room temperature and maintained for two hrs. The material is filtered washed with isopropyl acetate and water mixture and then dried at 50° C.-60° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07468442B2 |
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| Source dataset | uspto-grants-2008_12 |
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| ORD ID | ord-26a0341856334674ab40185ba9271787 |
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| Source note | uspto-grants-2008_12 |
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