Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Benzene | HCID 241 | — |
| Reactant | Caprolactam | HCID 7768 | — |
| Reactant | Bromine | HCID 24408 | — |
| Reactant | Phosphorus tribromide | HCID 24614 | — |
| Product | 3-Bromoazepan-2-one | HCID 11030635 | — |
Reaction Steps
A benzene (50 g; manufactured by JUNSEI CHEMICAL Co., Ltd.) solution in which 240 g (1.5 mol) of bromine (manufactured by JUNSEI CHEMICAL Co., Ltd.) were dissolved was cooled with ice to 10° C. To the cooled solution, 450 g (1.6 mol) of 90% phosphorus tribromide (manufactured by Wako Pure Chemical Industries Ltd.) were added while the temperature of the reaction solution was maintained at 10° C. or less, and the resultant reaction solution was stirred for 60 minutes. Into the reaction solution, a benzene (220 g) solution in which 85 g (0.75 mol) of commercially available 6-hexanolactam (trade name: ε-caprolactam; manufactured by Tokyo Chemical Industry Co., Ltd.) were dissolved was added dropwise through a dropping funnel over 30 minutes while maintaining the temperature of the reaction solution at 10° C. or less.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07902383B2 |
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| Source dataset | uspto-grants-2011_03 |
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| ORD ID | ord-89cec7fd60294543a8368e9f33174bd0 |
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| Source note | uspto-grants-2011_03 |
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