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2-Nitropropane → HCID 86686339, 화합물

HRID 1043906
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HRID 1043906 반응식
C[O-].[Na+].[N+](C(C)C)([O-])=[O:5].[Br:10][C:11]1[C:12]([CH2:19]Br)=[N:13][C:14]([CH3:18])=[CH:15][C:16]=1[CH3:17]>CO>[Br:10][C:11]1[C:12]([CH:19]=[O:5])=[N:13][C:14]([CH3:18])=[CH:15][C:16]=1[CH3:17]
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참가 물질

5

반응물 3

HCID 3982-NitropropaneHCID 10942334Sodium MethoxideHCID 86686337HCID 86686337, 화합물

생성물 1

HCID 86686339HCID 86686339, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Sodium methoxide (581 mg) was added to a solution of 2-nitropropane (0.982 mL) in methanol (20 mL) at room temperature, and the mixture was stirred at the same temperature for 20 minutes. 3-bromo-2-(bromomethyl)-4,6-dimethylpyridine obtained in Preparation Example 33(1) (1.00 g) was added to the reaction mixture, and the mixture was stirred at 50° C. for five hours. The reaction mixture was concentrated under reduced pressure, and water was added to the residue, followed by extraction with ethyl acetate. The organic layer was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate/n-heptane, 0% to 50%) to give the title compound (467 mg).

후처리

  1. additionwas added to the reaction mixture
  2. stirringthe mixture was stirred at 50° C. for five hours
  3. concentrationThe reaction mixture was concentrated under reduced pressure, and water
  4. additionwas added to the residue
  5. extractionfollowed by extraction with ethyl acetate
  6. concentrationThe organic layer was concentrated under reduced pressure
  7. customthe residue was purified by silica gel column chromatography (ethyl acetate/n-heptane, 0% to 50%)

출처 및 근거

ORD 기록
ord-929c0fab8bfb4ccca69569d10e4728d0
출처 데이터셋
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08563565B2

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