N-t-butyloxycarbonyl-3,5-dinitro-4-methylaniline → 4-Amino-2,6-Dinitrotoluene

HRID 618255

반응식

HRID 618255 반응식
C(OC([NH:8][C:9]1[CH:14]=[C:13]([N+:15]([O-:17])=[O:16])[C:12]([CH3:18])=[C:11]([N+:19]([O-:21])=[O:20])[CH:10]=1)=O)(C)(C)C>FC(F)(F)C(O)=O>[CH3:18][C:12]1[C:13]([N+:15]([O-:17])=[O:16])=[CH:14][C:9]([NH2:8])=[CH:10][C:11]=1[N+:19]([O-:21])=[O:20]

참가 물질

3

반응물 1

HCID 18789671N-t-butyloxycarbonyl-3,5-dinitro-4-methylaniline

생성물 1

HCID 295744-Amino-2,6-Dinitrotoluene수율 47.4%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

A mixture of N-t-butyloxycarbonyl-3,5-dinitro-4-methylaniline (7.8 g, from above) and trifluoroacetic acid (100 mL) was stirred at room temperature for 15 min. After evaporation of the solvent under reduced pressure, the residue was taken up in ethyl acetate (100 mL), washed with saturated sodium bicarbonate solution, half-saturated sodium chloride solution, and dried over magnesium sulfate. After evaporation of the solvent, the residue was purified by flash column chromatography on silica gel eluting with acetone:hexane (1:3) to give 4-methyl-3,5-dinitro-phenylamine (2.45 g).

후처리

  1. customAfter evaporation of the solvent under reduced pressure
  2. washwashed with saturated sodium bicarbonate solution, half-saturated sodium chloride solution
  3. dry with materialdried over magnesium sulfate
  4. customAfter evaporation of the solvent
  5. customthe residue was purified by flash column chromatography on silica gel eluting with acetone:hexane (1:3)

출처 및 근거

ORD 기록
ord-0f86b88d69c74c7798a463364e738130
출처 데이터셋
uspto-grants-1999_09
특허 번호
US05952362

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