Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | [1,1'-Biphenyl]-2-carbonyl chloride | HCID 12563768 | — |
| Reactant | HCID 22100007 | HCID 22100007 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22099835 | HCID 22099835 | 30.1% |
Reaction Steps
A mixture of 0.263 g of 10,11-dihydro-10(4-amino-2-chlorobenzoyl)dibenz[b,f][1,4]oxazepine, 0.195 g of [1,1'-bipheny]-2-carbonyl chloride and 0.116 g of N,N-diisopropylethylamine in 7 ml of dichloromethane is stirred at room temperature for 3 hours. The mixture is poured into water and extracted with dichloromethane. The extract is washed with 2N Na2CO3, water, brine and dried (Na2SO4). The solution is filtered through a thin pad of hydrous magnesium silicate (pad washed with dichloromethane). The filtrate is concentrated to dryness to give a yellow solid. The solid is purified by chromatography on thick layer silica gel plates with hexane-ethyl acetate (1:1) as solvent to give 0.12 g of a yellow glass, m.p. 145° C.-188° C.: Anal.found: C, 73.6; H, 4.6; N,5.0; Cl, 6.4.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05849735 |
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| Source dataset | uspto-grants-1998_12 |
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| ORD ID | ord-564e38eb06aa48af9e71a6d6bc36626b |
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| Source note | uspto-grants-1998_12 |
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