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m-Toluidine → HCID 69128102, 화합물

HRID 1960225
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HRID 1960225 반응식
C1COCC1.[C:6]1([S:12][CH:13]=[CH:14][C:15](Cl)=[O:16])[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[CH3:18][C:19]1[CH:20]=[C:21]([CH:23]=[CH:24][CH:25]=1)[NH2:22]>C(N(CC)CC)C>[CH3:18][C:19]1[CH:20]=[C:21]([NH:22][C:15](=[O:16])[CH:14]=[CH:13][S:12][C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=2)[CH:23]=[CH:24][CH:25]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7934m-ToluidineHCID 8028Tetrahydrofuran2회HCID 713526793-(Phenylsulfanyl)prop-2-enoyl chloride

생성물 1

HCID 69128102HCID 69128102, 화합물수율 85%

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

THF (45 ml) solution of 3-(phenylthio)acryloyl chloride (3.03 g) was added to THF (45 ml) solution of triethylamine (2.09 ml) under ice-cooling. 3-methylaniline (1.62 g) was added to the mixture under ice-cooling and stirred at room temperature for ten hours. The reaction solution was concentrated under reduced pressure. Ice cooled 1N hydrochloric acid (40 ml) and ethyl acetate (200 ml) were added to the residue and separated to two layer. The organic layer was washed with aqueous saturated sodium chloride solution (40 ml) twice, dried over anhydrous magnesium sulfate, filtered off inorganic salt and concentrated under reduced pressure to obtain N-(3-methylphenyl)-3-(phenylthio)acrylamide (3.46 g).

후처리

  1. temperaturecooling
  2. temperaturecooling
  3. concentrationThe reaction solution was concentrated under reduced pressure
  4. temperatureIce cooled 1N hydrochloric acid (40 ml) and ethyl acetate (200 ml)
  5. additionwere added to the residue
  6. customseparated to two layer
  7. washThe organic layer was washed with aqueous saturated sodium chloride solution (40 ml) twice
  8. dry with materialdried over anhydrous magnesium sulfate
  9. filtrationfiltered off inorganic salt
  10. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-288a46a6e2994819b85ed13aa11dcf5a
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08410316B2

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