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1H-1,2,4-Triazole → HCID 19043019, 화합물

HRID 1644847
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HRID 1644847 반응식
[OH-].[K+].[NH:3]1[CH:7]=[N:6][CH:5]=[N:4]1.[Br:8][C:9]1[CH:14]=[CH:13][C:12]([CH2:15]Br)=[CH:11][CH:10]=1>CN(C=O)C>[Br:8][C:9]1[CH:14]=[CH:13][C:12]([CH2:15][N:3]2[CH:7]=[N:6][CH:5]=[N:4]2)=[CH:11][CH:10]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 92571H-1,2,4-TriazoleHCID 14797Potassium HydroxideHCID 685274-Bromobenzyl bromide

생성물 1

HCID 19043019HCID 19043019, 화합물수율 62%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
0 °C

실험 절차

DMF and KOH (3.3 g, 58 mmol) were stirred together at rt for 5 minutes before adding 1,2,4-triazole (1 g, 14.5 mmol). After a further 30 minutes, the reaction mixture was cooled to 0° C. and 1-bromo-4-bromomethyl-benzene (7.2 g, 29 mmol) was added dropwise over 5 minutes. The reaction mixture was heated to 60° C., then cooled to rt, extracted with ethyl acetate and water, and subsequently dried over K2CO3. The solvent was evaporated to yield yellow-white crystals, which, upon repeated recrystallisation, (ethylacetate/isohexane) yielded 0.60 g of the sub-title compound as white crystals (62% isolated yield).

후처리

  1. temperatureThe reaction mixture was heated to 60° C.
  2. temperaturecooled to rt
  3. extractionextracted with ethyl acetate and water
  4. dry with materialsubsequently dried over K2CO3
  5. customThe solvent was evaporated
  6. customto yield yellow-white crystals, which
  7. customrecrystallisation, (ethylacetate/isohexane)

출처 및 근거

ORD 기록
ord-096deeaf47694ee9957c99f89c519336
출처 데이터셋
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08124638B2

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