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

HRID 1158149노트

반응식

HRID 1158149 반응식
[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]

참가 물질

5

반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-47545cc8b4ff45eea1b76ee1fe4c10f6
출처 데이터셋
uspto-grants-2010_10
특허 번호
US07807708B2

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