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Benzene → 2-(4-Phenylpiperidino)-ethyl 2-(3-nitrobenzylidene)acetoacetate

HRID 746248
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HRID 746248 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([CH:9]=[CH:10][CH:11]=1)[CH:7]=O)([O-:3])=[O:2].[C:12]([O:18][CH2:19][CH2:20][N:21]1[CH2:26][CH2:25][CH:24]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[CH2:23][CH2:22]1)(=[O:17])[CH2:13][C:14]([CH3:16])=[O:15].N1CCCCC1.C1C=CC=CC=1>O>[N+:1]([C:4]1[CH:5]=[C:6]([CH:9]=[CH:10][CH:11]=1)[CH:7]=[C:13]([C:14]([CH3:16])=[O:15])[C:12]([O:18][CH2:19][CH2:20][N:21]1[CH2:22][CH2:23][CH:24]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[CH2:25][CH2:26]1)=[O:17])([O-:3])=[O:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 241BenzeneHCID 74493-NitrobenzaldehydeHCID 8082PiperidineHCID 138611532-(4-Phenylpiperidino)ethyl acetoacetate

생성물 1

HCID 539264322-(4-Phenylpiperidino)-ethyl 2-(3-nitrobenzylidene)acetoacetate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of m-nitrobenzaldehyde (0.66 g), 2-(4-phenylpiperidino)ethyl acetoacetate (1.2 g), piperidine (0.1 ml) and benzene (20 ml) was refluxed overnight, during which time the water produced was removed azeotropically. The solvent was then distilled off and the residue was chromatographed on silica gel (50 g) [ethyl acetate-hexane (1:1, v/v)] to give 2-(4-phenylpiperidino)-ethyl 2-(3-nitrobenzylidene)acetoacetate as an oil. Yield 0.80 g (45.7%).

후처리

  1. customproduced
  2. customwas removed azeotropically
  3. distillationThe solvent was then distilled off
  4. customthe residue was chromatographed on silica gel (50 g) [ethyl acetate-hexane (1:1

출처 및 근거

ORD 기록
ord-b989c8e2d49a4d30a6c718b5c48d2aea
출처 데이터셋
uspto-grants-1986_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04603135

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