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

HRID 1085308ノート

反応式

HRID 1085308 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a8918bf02a3c494689d76a144cbbe8ef
出典データセット
uspto-grants-1991_04
特許番号
US05008389

反応ノート

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