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

반응식

HRID 1707576 반응식
[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

참가 물질

4

반응물 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

생성물 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-piperazinecarboxylate수율 43.8%

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-8896ec655f0f4652a1982053d00f9a88
출처 데이터셋
uspto-grants-1994_10
특허 번호
US05354746

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