Hydrochloric Acid → 2(3H)-Thiazolethione, 4-(chloromethyl)-3-(2,3,4-trifluorophenyl)-

HRID 1073803노트

반응식

HRID 1073803 반응식
[F:1][C:2]1[C:7]([F:8])=[C:6]([F:9])[CH:5]=[CH:4][C:3]=1[NH:10][C:11](=[S:18])[S:12][CH2:13][C:14](=O)[CH2:15][Cl:16].Cl>CO>[Cl:16][CH2:15][C:14]1[N:10]([C:3]2[CH:4]=[CH:5][C:6]([F:9])=[C:7]([F:8])[C:2]=2[F:1])[C:11](=[S:18])[S:12][CH:13]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 100869643-chloro-2-oxopropyl N-(2,3,4-trifluorophenyl)dithiocarbamate

생성물 1

HCID 41903592(3H)-Thiazolethione, 4-(chloromethyl)-3-(2,3,4-trifluorophenyl)-수율 69%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

3-Chloro-2-oxopropyl N-(2,3,4-trifluorophenyl)dithiocarbamate (4.0 g) prepared in the same manner as in Reference Example 6 was added to 30% HCl in methanol (15 ml) and the mixture was refluxed for 3 hours. The solvent was distilled off under reduced pressure and to the residue was added cooled water and the solution was extracted with chloroform. The extract was washed with a NaCl solution, dried over anhydrous sodium sulfate and the solvent was distilled off under reduced pressure. The residue was recrystallized from cyclohexane to give the title compound (2.6 g) as pale yellow crystals, m.p. 127°-130° C.

후처리

  1. temperaturethe mixture was refluxed for 3 hours
  2. distillationThe solvent was distilled off under reduced pressure and to the residue
  3. additionwas added
  4. temperaturecooled water
  5. extractionthe solution was extracted with chloroform
  6. washThe extract was washed with a NaCl solution
  7. dry with materialdried over anhydrous sodium sulfate
  8. distillationthe solvent was distilled off under reduced pressure
  9. customThe residue was recrystallized from cyclohexane

출처 및 근거

ORD 기록
ord-0fdd31c9ef7b41d3ac783f1bafd02c11
출처 데이터셋
uspto-grants-1990_11
특허 번호
US04971967

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