2-Chloro-5-nitropyridine → HCID 4418042, 화합물

HRID 1030997노트

반응식

HRID 1030997 반응식
Cl[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][N:3]=1>C(NCC)C.C(Cl)Cl>[CH2:2]([N:3]([CH2:4][CH3:5])[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][N:3]=1)[CH3:7]

참가 물질

4

반응물 1

HCID 783082-Chloro-5-nitropyridine

생성물 1

HCID 4418042HCID 4418042, 화합물수율 195.5%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8021Diethylamine용매

실험 절차

A stirred mixture of 27.6 g (0.174 mole) of 2-chloro-5-nitropyridine in 500 ml of diethylamine was heated at reflux for two days. The excess diethylamine was removed by distillation under reduced pressure, leaving a residue. This residue was dissolved in methylene chloride, and the organic solution was washed with an aqueous, 10% sodium hydroxide solution. The washed organic phase was dried over anhydrous magnesium sulfate and was filtered. The filtrate was evaporated under reduced pressure to yield 33.2 g of 2-diethylamino-5-nitropyridine as a solid. The nmr spectrum was consistent with the proposed structure.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for two days
  3. customThe excess diethylamine was removed by distillation under reduced pressure
  4. customleaving a residue
  5. washthe organic solution was washed with an aqueous, 10% sodium hydroxide solution
  6. dry with materialThe washed organic phase was dried over anhydrous magnesium sulfate
  7. filtrationwas filtered
  8. customThe filtrate was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-ce5c4d0c44d6447eb50a8d7463a72ce8
출처 데이터셋
uspto-grants-1992_04
특허 번호
US05108486

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