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

HRID 1506935노트

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HRID 1506935 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-7521691910cc4a899d01c0421784865d
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09221790B2

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