Diphenyl Ether → Ethyl 4-[2-(8-chlorodibenz[b,f][1,4]oxazepin-10(11H)-yl)-3,4-dioxo-1-cyclobuten-1-yl]-1-phenyl-2-piperazinecarboxylate

HRID 1707576

Reaktionsgleichung

Reaktionsgleichung von HRID 1707576
[Cl:1][C:2]1[CH:16]=[CH:15][C:5]2[O:6][C:7]3[CH:14]=[CH:13][CH:12]=[CH:11][C:8]=3[CH:9]=[N:10][C:4]=2[CH:3]=1.C([O:19][C:20]1[C:23](=[O:24])[C:22](=O)[C:21]=1[N:26]1[CH2:31][CH2:30][N:29]([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[CH:28]([C:38]([O:40][CH2:41][CH3:42])=[O:39])[CH2:27]1)C.C1(OC2C=CC=CC=2)C=CC=CC=1>>[Cl:1][C:2]1[CH:16]=[CH:15][C:5]2[O:6][C:7]3[CH:14]=[CH:13][CH:12]=[CH:11][C:8]=3[CH2:9][N:10]([C:22]3[C:23](=[O:24])[C:20](=[O:19])[C:21]=3[N:26]3[CH2:31][CH2:30][N:29]([C:32]4[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=4)[CH:28]([C:38]([O:40][CH2:41][CH3:42])=[O:39])[CH2:27]3)[C:4]=2[CH:3]=1

Komponenten

4

Edukt 3

HCID 7583Diphenyl EtherHCID 8382678-Chloro-dibenz[b,f]-[1,4]oxazepineHCID 18961721Ethyl 4-(2-ethoxy-3,4-dioxo-1-cyclobuten-1-yl)-1-phenyl-2-piperazinecarboxylate

Produkt 1

HCID 15232292Ethyl 4-[2-(8-chlorodibenz[b,f][1,4]oxazepin-10(11H)-yl)-3,4-dioxo-1-cyclobuten-1-yl]-1-phenyl-2-piperazinecarboxylateAusbeute 43,8 %

Versuchsvorschrift

A mixture of 8-chloro-dibenz[b,f][1,4]oxazepine (1.02 g) and the product of Example 3 (0.26 g) and diphenyl ether (3 mL) was heated to reflux for 1.75 hours. The mixture was rapidly filtered thourough a small column of silica gel and the filtrate was concentrated. The residue was purified by chromatography on silica gel to obtain the title compound (0.173 g).

Aufarbeitung

  1. temperatureto reflux for 1.75 hours
  2. filtrationThe mixture was rapidly filtered thourough a small column of silica gel
  3. concentrationthe filtrate was concentrated
  4. customThe residue was purified by chromatography on silica gel

Quellen und Nachweise

ORD-Eintrag
ord-8896ec655f0f4652a1982053d00f9a88
Quelldatensatz
uspto-grants-1994_10
Patentnummer
US05354746

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