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

反応式

HRID 1707576 の反応式
[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

参加物

4

反応物 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

生成物 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-piperazinecarboxylate収率 43.8%

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-8896ec655f0f4652a1982053d00f9a88
出典データセット
uspto-grants-1994_10
特許番号
US05354746

関連ノート

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