Acetic Acid → 2,5-difluoro-4-nitro-N-benzenesulphonylaniline

HRID 4235

반응식

HRID 4235 반응식
C(O)(=O)C.[N:5]([O-:7])=[O:6].[Na+].[F:9][C:10]1[CH:25]=[CH:24][C:23]([F:26])=[CH:22][C:11]=1[NH:12][S:13]([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)(=[O:15])=[O:14].[N+]([O-])(O)=O>O>[F:9][C:10]1[CH:25]=[C:24]([N+:5]([O-:7])=[O:6])[C:23]([F:26])=[CH:22][C:11]=1[NH:12][S:13]([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)(=[O:14])=[O:15]

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 944Nitric AcidHCID 8500589N-(2,5-difluorophenyl)benzenesulfonamideHCID 23668193Sodium Nitrite

생성물 1

HCID 201519862,5-difluoro-4-nitro-N-benzenesulphonylaniline

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
96 °C

실험 절차

To 310 ml of acetic acid diluted with 160 ml of water are added: 1.5 g of sodium nitrite, 0.16 mole (42 g) of 2,5-difluoro-N-benzenesulphonylaniline prepared in the previous stage and 0.94 mole (39 ml) of nitric acid (d=1.52). The reaction mixture is heated to 96° C. for 1 hour. After cooling it is poured onto 1 kg of ice and water. The expected product precipitates. After being filtered off and washed to neutrality it is recrystallized from 250 ml of acetic acid; it melts at 176° C.

후처리

  1. additionare added
  2. temperatureAfter cooling it
  3. customThe expected product precipitates
  4. filtrationAfter being filtered off
  5. washwashed
  6. customis recrystallized from 250 ml of acetic acid

출처 및 근거

ORD 기록
ord-6690a163904649839ee51f83c59f74e3
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04725283

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