Potassium Iodide → 1-[2-(4-methoxy-phenyl)-oxazol-4-ylmethyl]-1H-[1,2,3]triazole

HRID 854677노트

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HRID 854677 반응식
Cl[CH2:2][C:3]1[N:4]=[C:5]([C:8]2[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[CH:10][CH:9]=2)[O:6][CH:7]=1.[NH:16]1[CH:20]=[CH:19][N:18]=[N:17]1.[I-].[K+].[OH-].[Na+]>CC(O)(CC)C>[CH3:15][O:14][C:11]1[CH:12]=[CH:13][C:8]([C:5]2[O:6][CH:7]=[C:3]([CH2:2][N:16]3[CH:20]=[CH:19][N:18]=[N:17]3)[N:4]=2)=[CH:9][CH:10]=1

참가 물질

6

반응물 4

HCID 4875Potassium IodideHCID 14798Sodium HydroxideHCID 199587944-(Chloromethyl)-2-(4-methoxyphenyl)-1,3-oxazoleHCID 178418936HCID 178418936, 화합물

생성물 1

HCID 694249801-[2-(4-methoxy-phenyl)-oxazol-4-ylmethyl]-1H-[1,2,3]triazole수율 64%

시약·촉매·용매 1

HCID 64052-Methyl-2-butanol용매

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온도
120 °C

실험 절차

A suspension of 5.59 g (25 mmol) 4-chloromethyl-2-(4-methoxy-phenyl)-oxazole, 2.59 g (37.5 mmol) 1H-[1,2,3]triazole, 0.41 g (2.5 mmol) potassium iodide and 1.5 g (37.5 mmol) sodium hydroxide (NaOH) in 50 ml 2-methyl-2-butanol was stirred at 120° C. for 5 h. After evaporation, the residue was quenched with water and extracted with ethyl acetate. The extract was dried, concentrated and purified on silica. Elution with ethyl acetate yielded 4.1 g (64%) 1-[2-(4-methoxy-phenyl)-oxazol-4-ylmethyl]-1H-[1,2,3]triazole as white crystals, melting at 126-127° C.

후처리

  1. customAfter evaporation
  2. customthe residue was quenched with water
  3. extractionextracted with ethyl acetate
  4. customThe extract was dried
  5. concentrationconcentrated
  6. custompurified on silica
  7. washElution with ethyl acetate

출처 및 근거

ORD 기록
ord-659cccd970954677ac22b9dd361dfb45
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07259262B2

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