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Hydrogen Peroxide → 6-(4-Phenylsulfinyl-butoxy)-3,4-dihydro-carbostyril

HRID 1065311
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HRID 1065311 반응식
[OH:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[NH:8][C:7](=[O:12])[CH2:6][CH2:5]2.C(=O)([O-])[O-].[K+].[K+].[C:19]1([S:25]([CH2:27][CH2:28][CH2:29][CH2:30]Br)=[O:26])[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.C1(S)C=CC=CC=1.BrCCCCBr.OO>CS(C)=O.C(O)(=O)C.O>[C:19]1([S:25]([CH2:27][CH2:28][CH2:29][CH2:30][O:1][C:2]2[CH:3]=[C:4]3[C:9](=[CH:10][CH:11]=2)[NH:8][C:7](=[O:12])[CH2:6][CH2:5]3)=[O:26])[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1
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참가 물질

10

반응물 6

HCID 784Hydrogen PeroxideHCID 7969ThiophenolHCID 80561,4-DibromobutaneHCID 11430Potassium CarbonateHCID 27740406-Hydroxy-3,4-dihydro-2(1H)-quinolinoneHCID 545301224-Phenylsulfinylbutylbromide

생성물 1

HCID 13138341
6-(4-Phenylsulfinyl-butoxy)-3,4-dihydro-carbostyril

시약·촉매·용매 3

HCID 176Acetic Acid용매HCID 679Dimethyl Sulfoxide용매HCID 962Water용매

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온도
25 °C

실험 절차

32.6 gm (0.2 mol) of 6-hydroxy-3,4-dihydro-carbostyril [see F. F. Mayer et al., Ber. Dtsch. Chem. Ges. 60, 858 (1927)] and 27.6 gm (0.2 mol) of potassium carbonate were stirred for 5 minutes in 600 ml of dimethylsulfoxide which had been dried over a molecular sieve, and then 52.2 gm of 4-phenylsulfinyl-butyl bromide (0.2 mol) (prepared from thiophenol and 1,4-dibromo-butane and subsequent oxidation with hydrogen peroxide in glacial acetic acid analogous to Example 2; oily substance, solidified upon standing in the refrigerator) were added. After stirring it for 15 hours at 25° C., the reaction mixture was poured into 6 liters of water. After stirring the aqueous mixture for 30 minutes more, the precipitated product was suction-filtered off and thoroughly washed with water. After drying, the filter cake was recrystallized from about 600 ml of xylene in the presence of charcoal. White crystals with a melting point of 144.5°-145.5° C. were obtained.

후처리

  1. customhad been dried over a molecular sieve
  2. additionwere added
  3. stirringAfter stirring the aqueous mixture for 30 minutes more
  4. filtrationthe precipitated product was suction-filtered off
  5. washthoroughly washed with water
  6. customAfter drying
  7. customthe filter cake was recrystallized from about 600 ml of xylene in the presence of charcoal
  8. customWhite crystals with a melting point of 144.5°-145.5° C. were obtained

출처 및 근거

ORD 기록
ord-813757f1bf554df4b45e6958d15c5ea1
출처 데이터셋
uspto-grants-1982_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04329347

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