Triethylamine → 3-(1,2,3-Triazol-1-yl)propyl methanesulfonate

HRID 1506935ノート

反応式

HRID 1506935 の反応式
[N:1]1([CH2:6][CH2:7][CH2:8][OH:9])[CH:5]=[CH:4][N:3]=[N:2]1.C(N(CC)CC)C.[CH3:17][S:18](Cl)(=[O:20])=[O:19]>ClCCl>[CH3:17][S:18]([O:9][CH2:8][CH2:7][CH2:6][N:1]1[CH:5]=[CH:4][N:3]=[N:2]1)(=[O:20])=[O:19]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 220309141-(3-Hydroxypropyl)-1,2,3-triazole

生成物 1

HCID 866805493-(1,2,3-Triazol-1-yl)propyl methanesulfonate収率 75%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

3-(1,2,3-triazol-1-yl)propanol (2.5 g, 19.66 mmol) was dissolved in dichloromethane (50 mL), and the solution was cooled to 0° C. Then, triethylamine (5.53 mL, 39.32 mmol) and methane sulfonyl chloride (2.3 mL, 29.5 mmol) were added thereto. The reaction mixture was warmed to room temperature, stirred for 2 hours, extracted with dichloromethane and water, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The resulting residue was purified by column chromatography to afford the title compound (3.01 g, 75%).

後処理

  1. temperatureThe reaction mixture was warmed to room temperature
  2. extractionextracted with dichloromethane and water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe resulting residue was purified by column chromatography

出典と根拠

ORDレコード
ord-7521691910cc4a899d01c0421784865d
出典データセット
uspto-grants-2015_12
特許番号
US09221790B2

反応ノート

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