Potassium Carbonate → HCID 14650107, 화합물

HRID 248911노트

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HRID 248911 반응식
[CH:1]([O:5][C:6]1[CH:11]=[CH:10][C:9]([OH:12])=[CH:8][CH:7]=1)([CH2:3][CH3:4])[CH3:2].C(=O)([O-])[O-].[K+].[K+].[Br:19][C:20]1[S:24][C:23]([CH2:25]Cl)=[CH:22][CH:21]=1>CN(C)C=O>[CH:1]([O:5][C:6]1[CH:7]=[CH:8][C:9]([O:12][CH2:25][C:23]2[S:24][C:20]([Br:19])=[CH:21][CH:22]=2)=[CH:10][CH:11]=1)([CH2:3][CH3:4])[CH3:2]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 101982272-bromo-5-(chloromethyl)thiopheneHCID 138820044-(1-Methyl-1-propyloxy)-phenol

생성물 1

HCID 14650107HCID 14650107, 화합물수율 46.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

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온도
20 °C

실험 절차

6.64 g of 4-(sec-butyloxy)-phenol and 5.52 g of potassium carbonate are heated in 50 ml of anhydrous dimethylformamide for one hour at 70° C. Subsequently, 8.46 g of 5-bromo-2-chloromethylthiophene in 20 ml anhydrous dimethylformamide is dripped in. The mixture is stirred for 6 hours at 80° C. and overnight at room temperature (about 20° C.). It is then poured into 100 ml of ice water and extracted three times with ethyl acetate, and the organic phases are dried over magnesium sulfate. The solvent is evaporated off to give a crude product which is purified by chromatography on silica gel using n-hexane/ethyl acetate (4:1) as eluant. There is obtained 6.3 g of 2-[4-(sec-butyloxy)-phenoxymethyl]-5-bromothiophene as a colorless oil.

후처리

  1. extractionextracted three times with ethyl acetate
  2. dry with materialthe organic phases are dried over magnesium sulfate
  3. customThe solvent is evaporated off
  4. customto give a crude product which
  5. customis purified by chromatography on silica gel

출처 및 근거

ORD 기록
ord-5c4afa871395412c8915faf18e66e2f6
출처 데이터셋
uspto-grants-1993_05
특허 번호
US05212194

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