Methyl iodide → 5-Bromo-2-(methylthio)benzo[d]thiazole

HRID 1619261ノート

反応式

HRID 1619261 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[S:9][C:8]([SH:10])=[N:7][C:6]=2[CH:11]=1.[CH2:12](N(CC)CC)C.CI>CCO>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[S:9][C:8]([S:10][CH3:12])=[N:7][C:6]=2[CH:11]=1

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 8471TriethylamineHCID 178527757HCID 178527757、化合物

生成物 1

HCID 28012715-Bromo-2-(methylthio)benzo[d]thiazole収率 80%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 5-bromobenzo[d]thiazole-2-thiol (24 mg, 0.098 mmol) in EtOH (1.5 mL) was added triethylamine (10 mg, 0.098 mmol) and methyliodide (14 mg, 0.098 mmol). The mixture was heated at reflux for 1.5 h. Then the mixture was extracted with dichloromethane (3×10 mL). The combined organic extracts were washed with brine, dried (Na2SO4) and concentrated to give 5-bromo-2-(methylthio)benzothiazole 20 mg (80%).

後処理

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 1.5 h
  3. extractionThen the mixture was extracted with dichloromethane (3×10 mL)
  4. washThe combined organic extracts were washed with brine
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-0fd5e26727fa4100a1249daf4ff7215e
出典データセット
uspto-grants-2014_07
特許番号
US08772285B2

反応ノート

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