Cesium carbonate → Ethyl 3''-tert-butyl-4-[4-(tert-butyldimethylsilanyloxy)butoxy]-4''-diethylamino[1,1';3',1'']terphenyl-4-carboxylate

HRID 1158149ノート

反応式

HRID 1158149 の反応式
[C:1]([C:5]1[CH:6]=[C:7]([C:16]2[CH:17]=[C:18]([C:23]3[CH:28]=[CH:27][C:26]([C:29]([O:31][CH2:32][CH3:33])=[O:30])=[CH:25][CH:24]=3)[CH:19]=[CH:20][C:21]=2O)[CH:8]=[CH:9][C:10]=1[N:11]([CH2:14][CH3:15])[CH2:12][CH3:13])([CH3:4])([CH3:3])[CH3:2].C(=O)([O-])[O-:35].[Cs+].[Cs+].Br[CH2:41][CH2:42][CH2:43][CH2:44][O:45][Si:46]([C:49]([CH3:52])([CH3:51])[CH3:50])([CH3:48])[CH3:47]>CN(C)C=O>[C:1]([C:5]1[CH:6]=[C:7]([C:16]2[CH:17]=[C:18]([C:23]3[CH:24]=[CH:25][C:26]([O:35][CH2:41][CH2:42][CH2:43][CH2:44][O:45][Si:46]([C:49]([CH3:52])([CH3:51])[CH3:50])([CH3:48])[CH3:47])([C:29]([O:31][CH2:32][CH3:33])=[O:30])[CH2:27][CH:28]=3)[CH:19]=[CH:20][CH:21]=2)[CH:8]=[CH:9][C:10]=1[N:11]([CH2:14][CH3:15])[CH2:12][CH3:13])([CH3:2])([CH3:4])[CH3:3]

参加物

5

反応物 3

HCID 10796Cesium carbonateHCID 582370(4-Bromobutoxy)(tert-butyl)dimethylsilaneHCID 11676663Ethyl 3''-tert-butyl-4''-diethylamino-4'-hydroxy[1,1';3',1'']terphenyl-4-carboxylate

生成物 1

HCID 86617895Ethyl 3''-tert-butyl-4-[4-(tert-butyldimethylsilanyloxy)butoxy]-4''-diethylamino[1,1';3',1'']terphenyl-4-carboxylate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

1 g of ethyl 3″-tert-butyl-4″-diethylamino-4′-hydroxy[1,1′;3′,1″]terphenyl-4-carboxylate obtained in Example 1d (2.2 mmol) are dissolved in 20 mL of dimethylformamide under a nitrogen atmosphere. 880 mg (2.7 mmol) of caesium carbonate are added. The reaction medium stirred at room temperature turns yellow. 0.64 mL of 1-bromo-4-(tert-butyldimethylsilanyloxy)butane (2.4 mmol) is then added and the reaction medium is heated at 80° C. for 18 hours. The reaction medium is then cooled to room temperature and then filtered. The solvents are evaporated off and the residue obtained is purified by chromatography on silica gel (eluent: 70/30 heptane/ethyl acetate).

後処理

  1. temperaturethe reaction medium is heated at 80° C. for 18 hours
  2. temperatureThe reaction medium is then cooled to room temperature
  3. filtrationfiltered
  4. customThe solvents are evaporated off
  5. customthe residue obtained
  6. customis purified by chromatography on silica gel (eluent: 70/30 heptane/ethyl acetate)

出典と根拠

ORDレコード
ord-47545cc8b4ff45eea1b76ee1fe4c10f6
出典データセット
uspto-grants-2010_10
特許番号
US07807708B2

反応ノート

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