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Water → 4-(Bromomethyl)-5-methyl-2-phenyl-2H-1,2,3-triazole

HRID 538613
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인쇄 미리보기

반응식

HRID 538613 반응식
[CH3:1][C:2]1[C:3]([CH2:13]O)=[N:4][N:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[N:6]=1.P(Br)(Br)[Br:16].O>C1(C)C=CC=CC=1>[Br:16][CH2:13][C:3]1[C:2]([CH3:1])=[N:6][N:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[N:4]=1
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참가 물질

5

반응물 3

HCID 962WaterHCID 24614Phosphorus tribromideHCID 563195(5-Methyl-2-phenyl-2H-1,2,3-triazol-4-yl)methanol

생성물 1

HCID 3387104-(Bromomethyl)-5-methyl-2-phenyl-2H-1,2,3-triazole수율 91.5%

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
120 °C

실험 절차

To a solution of (5-Methyl-2-phenyl-2H-[1,2,3]triazol-4-yl)-methanol (0.25 g, 1.30 mmol) in 10 ml of toluene was added PBr3 (0.53 g, 1.90 mmol) and the reaction mixture was heated at 120° C. for 20 min under nitrogen atmosphere. After the completion of the reaction mixture (TLC monitoring), water (25 mL) was added and extracted with ethyl acetate (3×50 mL). The combined organics was washed with water, brine, dried (Na2SO4), filtered and concentrated to get the desired product (0.30 g, 90%) as a yellow solid.

후처리

  1. extractionextracted with ethyl acetate (3×50 mL)
  2. washThe combined organics was washed with water, brine
  3. dry with materialdried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-229e93b492fd4c7a8525b4aaebeb2c53
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08865736B2

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