Sulfuric Acid → 2,5-Difluoro-4-nitroaniline

HRID 2258618노트

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HRID 2258618 반응식
CC1C=CC(S([NH:11][C:12]2[CH:17]=[C:16]([F:18])[C:15]([N+:19]([O-:21])=[O:20])=[CH:14][C:13]=2[F:22])(=O)=O)=CC=1.S(=O)(=O)(O)O>O>[F:22][C:13]1[CH:14]=[C:15]([N+:19]([O-:21])=[O:20])[C:16]([F:18])=[CH:17][C:12]=1[NH2:11]

참가 물질

4

반응물 2

HCID 1118Sulfuric AcidHCID 22921537N-(4-methylphenylsulfonyl)-2,5-difluoro-4-nitroaniline

생성물 1

HCID 2359302,5-Difluoro-4-nitroaniline수율 143.6%

시약·촉매·용매 1

HCID 962Water용매

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온도
90 °C

실험 절차

A stirred solution of 25.0 grams (0.076 mole) of N-(4-methylphenylsulfonyl)-2,5-difluoro-4-nitroaniline in 50 mL of water was cooled in an ice-water bath, and 150 mL of concentrated sulfuric acid was carefully added portionwise. Upon completion of the addition, the reaction mixture was heated to about 90° C., where it stirred for about four hours. The reaction mixture was then cooled and poured into wet ice. The resultant solid was collected by filtration and dried, yielding about 19.0 grams of 2,5-difluoro-4-nitroaniline. The NMR spectrum was consistent with the proposed structure.

후처리

  1. additionUpon completion of the addition
  2. temperatureThe reaction mixture was then cooled
  3. additionpoured into wet ice
  4. filtrationThe resultant solid was collected by filtration
  5. customdried

출처 및 근거

ORD 기록
ord-6e62b75be3694c899a13ab85019d3e76
출처 데이터셋
uspto-grants-1997_08
특허 번호
US05661108

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