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m-Chloroperbenzoic acid → 4-Allyloxy-8-(2-benzimidazolyl)sulfinyl-3-methyl-5,6,7,8-tetrahydroquinoline

HRID 1638587
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HRID 1638587 반응식
[CH2:1]([O:4][C:5]1[C:14]2[CH2:13][CH2:12][CH2:11][CH:10]([S:15][C:16]3[NH:17][C:18]4[CH:24]=[CH:23][CH:22]=[CH:21][C:19]=4[N:20]=3)[C:9]=2[N:8]=[CH:7][C:6]=1[CH3:25])[CH:2]=[CH2:3].ClC1C=CC=C(C(OO)=[O:34])C=1>C(Cl)Cl>[CH2:1]([O:4][C:5]1[C:14]2[CH2:13][CH2:12][CH2:11][CH:10]([S:15]([C:16]3[NH:20][C:19]4[CH:21]=[CH:22][CH:23]=[CH:24][C:18]=4[N:17]=3)=[O:34])[C:9]=2[N:8]=[CH:7][C:6]=1[CH3:25])[CH:2]=[CH2:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 141555244-Allyloxy-8(2-benzimidazolyl)thio-3-methyl-5,6,7,8-tetrahydroquinoline

생성물 1

HCID 141555644-Allyloxy-8-(2-benzimidazolyl)sulfinyl-3-methyl-5,6,7,8-tetrahydroquinoline

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

0.7 Gram of 4-allyloxy-8(2-benzimidazolyl)thio-3-methyl-5,6,7,8-tetrahydroquinoline was dissolved in 30 ml of methylene chloride, then this solution was cooled to -50° to -60° C., next to this solution was added dropwise a solution prepared by dissolving 0.43 g of 80%-meta-chloroperbenzoic acid in 10 ml of methylene chloride, and the reaction mixture was stirred for 20 minutes at the above-mentioned temperature. After the reaction was completed, the reaction mixture was washed with as aqueous solution of sodium carbonate, and dried with anhydrous magnesium sulfate. Methylene chloride was removed by evaporation under reduced pressure, the residue thus obtained was recrystallized from diethyl ether to obtain 0.4 g of 4-allyloxy-8-(2-benzimidazolyl)sulfinyl-3-methyl-5,6,7,8-tetrahydroquinoline. White powdery crystals. Melting point: 100°-102° C. (decomposed)

후처리

  1. temperaturethis solution was cooled to -50° to -60° C., next to this solution
  2. additionwas added dropwise a solution
  3. customprepared
  4. washthe reaction mixture was washed with as aqueous solution of sodium carbonate
  5. dry with materialdried with anhydrous magnesium sulfate
  6. customMethylene chloride was removed by evaporation under reduced pressure
  7. customthe residue thus obtained
  8. customwas recrystallized from diethyl ether

출처 및 근거

ORD 기록
ord-8f9606ec32e74485831454e0eb09233e
출처 데이터셋
uspto-grants-1989_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04880815

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