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Azobisisobutyronitrile → 5-Bromomethyl-4-(4-chlorophenyl)-2-methyloxazole

HRID 1982432
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반응식

HRID 1982432 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:9]=[C:10]([CH3:14])[O:11][C:12]=2[CH3:13])=[CH:4][CH:3]=1.[Br:15]N1C(=O)CCC1=O.N(C(C)(C)C#N)=NC(C)(C)C#N>C(Cl)(Cl)(Cl)Cl>[Br:15][CH2:13][C:12]1[O:11][C:10]([CH3:14])=[N:9][C:8]=1[C:5]1[CH:4]=[CH:3][C:2]([Cl:1])=[CH:7][CH:6]=1
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참가 물질

5

반응물 3

HCID 6547AzobisisobutyronitrileHCID 67184N-bromobutanimideHCID 11160071Oxazole, 4-(4-chlorophenyl)-2,5-dimethyl-

생성물 1

HCID 132932935-Bromomethyl-4-(4-chlorophenyl)-2-methyloxazole

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

실험 절차

A solution of 4-(4-chlorophenyl)-2,5-dimethyloxazole (6.21 g), N-bromosuccinimide (5.34 g) and azobisisobutyronitrile (0.25 g) in carbon tetrachloride (90 ml) was refluxed with stirring for 15 minutes, then washed with water, saturated aqueous sodium hydrogen carbonate and water in that order, and dried over anhydrous magnesium sulfate. The solvent was then distilled off and the residue was crystallized from cold ethanol to give 5-bromomethyl-4-(4-chlorophenyl)-2-methyloxazole, yield 6.73 g (78.4%). Recrystallization from ethanol gave needles, melting at 75°-76° C.

후처리

  1. washwashed with water, saturated aqueous sodium hydrogen carbonate and water in that order
  2. dry with materialdried over anhydrous magnesium sulfate
  3. distillationThe solvent was then distilled off
  4. customthe residue was crystallized from cold ethanol

출처 및 근거

ORD 기록
ord-39e7788ed2e845adb0303efd9a11125e
출처 데이터셋
uspto-grants-1986_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04596816

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