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

HRID 1944687ノート

反応式

HRID 1944687 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-45a1b769159946da840d57a52d26c256
出典データセット
uspto-grants-2013_03
特許番号
US08394842B2

反応ノート

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