Hydrofluoric Acid → 4-Methyl-thioanisol-2-thiocarboxylic acid amide

HRID 436311

반응식

HRID 436311 반응식
[S-:1][C:2]#[N:3].[K+].[CH3:5][C:6]1[CH:11]=[CH:10][C:9]([S:12][CH3:13])=[CH:8][CH:7]=1.F>>[CH3:5][C:6]1[CH:7]=[C:8]([C:2](=[S:1])[NH2:3])[C:9]([S:12][CH3:13])=[CH:10][CH:11]=1

참가 물질

4

반응물 3

HCID 14917Hydrofluoric AcidHCID 69334Benzene, 1-methyl-4-(methylthio)-2회HCID 516872Potassium thiocyanate

생성물 1

HCID 867345004-Methyl-thioanisol-2-thiocarboxylic acid amide

실험 절차

At a temperature and in the manner as indicated in Example 1, 39 g of potassium thiocyanate (0.4 mol) and 46 g of 4-methyl-thioanisol (0.33 mol) are stirred with 0.3 l of 98% hydrofluoric acid. The mixture is then stirred first for 10 hours at room temperature and then for 3 hours in a steel autoclave at 40° - 50° C, subsequently cooled, the reaction mixture is poured onto ice, the 4-methyl-thioanisol-2-thiocarboxylic acid amide precipitated is suction-filtered and dried. The yield (54 g) is 81% of the theoretical yield, relative to the 4-methyl-thioanisol used. After recrystallization of the product from chlorobenzene, the melting point is 160° C.

후처리

  1. temperaturesubsequently cooled
  2. additionthe reaction mixture is poured onto ice
  3. customthe 4-methyl-thioanisol-2-thiocarboxylic acid amide precipitated
  4. filtrationis suction-filtered
  5. customdried
  6. customThe yield (54 g)
  7. customAfter recrystallization of the product from chlorobenzene

출처 및 근거

ORD 기록
ord-266a05c8812e488eb5748f512d847a27
출처 데이터셋
uspto-grants-1977_02
특허 번호
US04008264

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