Iodoethane → 2-(Ethylthio)benzothiazole

HRID 1029361

反応式

HRID 1029361 の反応式
[SH:1][C:2]1[S:3][C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=1.[CH2:11](N(CC)CC)[CH3:12].ICC>>[CH2:11]([S:1][C:2]1[S:3][C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=1)[CH3:12]

参加物

4

反応物 3

HCID 6340IodoethaneHCID 8471TriethylamineHCID 178418395HCID 178418395、化合物

生成物 1

HCID 759932-(Ethylthio)benzothiazole収率 56%

実験手順

2-Mercaptobenzothiazole (16.72 g, 0.1 mol) in 52 ml 95% alcohol was reacted with 10.1 g (0.1 mol) triethylamine to give a brown solution. Iodoethane (15.6 g, 0.1 mol) was added and the mixture refluxed 45 minutes. The mixture was cooled and the solvent removed by rotary evaporation. Water (100 ml) was added to the residue and an oil separated. The aqueous phase was extracted 2×50 ml methylene chloride, the combined organic phases washed with 50 ml water, and then dried over Na2SO4. Filtration and rotary evaporation yielded a brown liquid which was distilled at 140°-141.5° C. (0.15 mm) to give 10.87 g (56%) pale yellow liquid.

後処理

  1. customto give a brown solution
  2. temperaturethe mixture refluxed 45 minutes
  3. temperatureThe mixture was cooled
  4. customthe solvent removed by rotary evaporation
  5. additionWater (100 ml) was added to the residue
  6. customan oil separated
  7. extractionThe aqueous phase was extracted 2×50 ml methylene chloride
  8. washthe combined organic phases washed with 50 ml water
  9. dry with materialdried over Na2SO4
  10. filtrationFiltration and rotary evaporation
  11. customyielded a brown liquid which
  12. distillationwas distilled at 140°-141.5° C. (0.15 mm)

出典と根拠

ORDレコード
ord-b866da13e881456c9d4d49c821dba5f1
出典データセット
uspto-grants-1992_04
特許番号
US05102781

関連ノート

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