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Potassium Carbonate → bis[6-{4-[(1E)-3-(4-pentyloxyphenoxy)-3-oxoprop-1-enyl]phenoxy}hexyl]2,2 bis(4-nitrobenzyl)malonate

HRID 2246021
ノート
印刷プレビュー

反応式

HRID 2246021 の反応式
Cl[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][O:8][C:9](=[O:41])[C:10]([CH2:31][C:32]1[CH:37]=[CH:36][C:35]([N+:38]([O-:40])=[O:39])=[CH:34][CH:33]=1)([CH2:21][C:22]1[CH:27]=[CH:26][C:25]([N+:28]([O-:30])=[O:29])=[CH:24][CH:23]=1)[C:11]([O:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19]Cl)=[O:12].[OH:42][C:43]1[CH:48]=[CH:47][C:46](/[CH:49]=[CH:50]/[C:51]([O:53][C:54]2[CH:59]=[CH:58][C:57]([O:60][CH2:61][CH2:62][CH2:63][CH2:64][CH3:65])=[CH:56][CH:55]=2)=[O:52])=[CH:45][CH:44]=1.[C:66](=[O:69])([O-])[O-:67].[K+].[K+]>[I-].C([N+](CCCC)(CCCC)CCCC)CCC.CC(=O)CC>[CH2:61]([O:60][C:57]1[CH:56]=[CH:55][C:54]([O:53][C:51](=[O:52])/[CH:50]=[CH:49]/[C:46]2[CH:45]=[CH:44][C:43]([O:42][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][O:8][C:9](=[O:41])[C:10]([CH2:31][C:32]3[CH:37]=[CH:36][C:35]([N+:38]([O-:40])=[O:39])=[CH:34][CH:33]=3)([CH2:21][C:22]3[CH:27]=[CH:26][C:25]([N+:28]([O-:30])=[O:29])=[CH:24][CH:23]=3)[C:11]([O:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][O:42][C:43]3[CH:44]=[CH:45][C:46](/[CH:49]=[CH:50]/[C:66]([O:67][C:54]4[CH:55]=[CH:56][C:57]([O:60][CH2:61][CH2:62][CH2:63][CH2:64][CH3:65])=[CH:58][CH:59]=4)=[O:69])=[CH:47][CH:48]=3)=[O:12])=[CH:48][CH:47]=2)=[CH:59][CH:58]=1)[CH2:62][CH2:63][CH2:64][CH3:65]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 59217445Bis[6-chlorohexyl]2,2 bis(4-nitrobenzyl)malonateHCID 592174494-pentoxyphenyl (2E)-3-{4-hydroxyphenyl}acrylate

生成物 1

HCID 59217452bis[6-{4-[(1E)-3-(4-pentyloxyphenoxy)-3-oxoprop-1-enyl]phenoxy}hexyl]2,2 bis(4-nitrobenzyl)malonate収率 65.7%

試薬・触媒・溶媒 2

HCID 67553
Tetrabutylammonium Iodide
触媒
HCID 6569Methyl Ethyl Ketone溶媒

実験手順

2.80 g (4.6 mmol) bis[6-chlorohexyl]2,2 bis(4-nitrobenzyl)malonate, 3.0 g (9.2 mmol) 4-pentoxyphenyl (2E)-3-{4-hydroxyphenyl}acrylate and 0.17 g (0.46 mmol) tetrabutylammonium iodide were dissolved in 30 ml 2-butanone. 2.53 g (18.3 mmol) potassium carbonate were added. The resulting suspension was heated at refluxing temperature and allowed to react for 48 h. After cooling to room temperature, the reaction mixture was partitioned between ethyl acetate and water. The organic phase was washed repeatedly with water, dried over sodium sulfate, filtered and concentrated by rotary evaporation to yield 3.6 g bis[6-{4-[(1E)-3-(4-pentyloxyphenoxy)-3-oxoprop-1-enyl]phenoxy}hexyl]2,2 bis(4-nitrobenzyl)malonate.

後処理

  1. temperatureThe resulting suspension was heated
  2. temperatureat refluxing temperature
  3. customto react for 48 h
  4. customthe reaction mixture was partitioned between ethyl acetate and water
  5. washThe organic phase was washed repeatedly with water
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated by rotary evaporation

出典と根拠

ORDレコード
ord-ce48a12435f341ad8e83dfeb50492dd5
出典データセット
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07687118B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート