2-Methoxyethylamine → 3-bromo-N-(2-methoxyethyl)-5-nitropyridin-2-amine

HRID 340471노트

반응식

HRID 340471 반응식
C(N(CC)CC)C.[CH3:8][O:9][CH2:10][CH2:11][NH2:12].O1CCCC1.[Br:18][C:19]1[C:20](Cl)=[N:21][CH:22]=[C:23]([N+:25]([O-:27])=[O:26])[CH:24]=1>O>[Br:18][C:19]1[C:20]([NH:12][CH2:11][CH2:10][O:9][CH3:8])=[N:21][CH:22]=[C:23]([N+:25]([O-:27])=[O:26])[CH:24]=1

참가 물질

6

반응물 4

HCID 80182-MethoxyethylamineHCID 8028TetrahydrofuranHCID 8471TriethylamineHCID 2308893-Bromo-2-chloro-5-nitropyridine

생성물 1

HCID 795353203-bromo-N-(2-methoxyethyl)-5-nitropyridin-2-amine수율 134%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Triethylamine (53 μl) and 2-methoxyethylamine (23 mg) were added to a tetrahydrofuran (2 ml) solution containing 3-bromo-2-chloro-5-nitropyridine (60 mg), followed by stirring at room temperature for 1 hour. Water was added to the reaction solution, followed by extraction with ethyl acetate. The resultant was washed with saturated saline and dried over anhydrous sodium sulfate. Subsequently, the solvent was distilled away under reduced pressure, the obtained residue was purified by silica gel chromatography (n-hexane:ethyl acetate=6:1 to 3:1), and a light yellow solid of 3-bromo-N-(2-methoxyethyl)-5-nitropyridin-2-amine (93.5 mg) was thus obtained.

후처리

  1. extractionfollowed by extraction with ethyl acetate
  2. washThe resultant was washed with saturated saline
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationSubsequently, the solvent was distilled away under reduced pressure
  5. customthe obtained residue was purified by silica gel chromatography (n-hexane:ethyl acetate=6:1 to 3:1)

출처 및 근거

ORD 기록
ord-6bacd450bdf6420f91e663be831853fd
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08895585B2

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