Sodium Hydroxide → HCID 59334623, 화합물

HRID 1639740노트

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HRID 1639740 반응식
[N+:1]([C:4]1C=C([N+]([O-])=O)C=C[C:5]=1[O-])([O-])=O.[NH2:14][N+:15]1[CH:20]=[CH:19][CH:18]=[C:17]([CH2:21][OH:22])[CH:16]=1.[OH-].[Na+]>C(#N)C>[CH3:5][C:4]1[N:1]=[C:16]2[C:17]([CH2:21][OH:22])=[CH:18][CH:19]=[CH:20][N:15]2[N:14]=1

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 866419191-Amino-3-(hydroxymethyl)pyridinium 2,4-dinitrobenzenolate

생성물 1

HCID 59334623HCID 59334623, 화합물수율 29%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a solution of 1-amino-3-(hydroxymethyl)pyridinium 2,4-dinitrobenzenolate (100 g, 323 mmol) in acetonitrile (1.08 L), was added 2 N sodium hydroxide (485 mL) at room temperature, and the mixture was stirred for 12 hr. Acetonitrile was evaporated under reduced pressure, and the residual aqueous solution was extracted with 3 times with chloroform. The extract was dried over anhydrous sodium sulfate and the solvent was evaporated under reduced pressure. The residue was purified by recrystallization (ethyl acetate/hexane) to give the title compound (14.0 g, yield 29%).

후처리

  1. customAcetonitrile was evaporated under reduced pressure
  2. extractionthe residual aqueous solution was extracted with 3 times with chloroform
  3. dry with materialThe extract was dried over anhydrous sodium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. customThe residue was purified by recrystallization (ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-bdf46ed98c9c446f8c8f067321182f2f
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08110585B2

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