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Water → 5,6-Dimethyl-2-methoxy-3-nitropyridine

HRID 1994235
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HRID 1994235 반응식
C[O-].[Na+].Cl[C:5]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][C:8]([CH3:14])=[C:7]([CH3:15])[N:6]=1.[CH2:16]([O:18]CC)C.O>CO>[CH3:14][C:8]1[CH:9]=[C:10]([N+:11]([O-:13])=[O:12])[C:5]([O:18][CH3:16])=[N:6][C:7]=1[CH3:15]
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참가 물질

6

반응물 4

HCID 962WaterHCID 3283Diethyl EtherHCID 100811492-Chloro-5,6-dimethyl-3-nitropyridineHCID 10942334Sodium Methoxide

생성물 1

HCID 222664775,6-Dimethyl-2-methoxy-3-nitropyridine수율 82.6%

시약·촉매·용매 1

HCID 887Methanol용매2회

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온도
50 °C

실험 절차

To a solution of 28% sodium methoxide (1.11 mL) and methanol (5.5 mL) was added dropwise a solution of 2-chloro-5,6-dimethyl-3-nitropyridine (1-013-05) (837 mg) in methanol (6.6 mL) for 5 min at room temperature under nitrogen atmosphere, and the reaction mixture was heated with stirring, in oil-bath at 50° C. for 7 h. To the reaction mixture was added diethyl ether and the reaction mixture was poured into water, extracted with twice with diethyl ether, washed once with water, and dried over magnesium sulfate. The solvent was evaporated under reduced pressure to give 5,6-dimethyl-2-methoxy-3-nitropyridine (1-013-06) (675 mg, 82.6%, m.p.: 71-73° C.) as an orange crystal.

후처리

  1. temperaturethe reaction mixture was heated
  2. extractionextracted with twice with diethyl ether
  3. washwashed once with water
  4. dry with materialdried over magnesium sulfate
  5. customThe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-68a7cbf7ccf240e9b88492f8affd65a8
출처 데이터셋
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07652141B2

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