Nitric Acid → 2'-Nitro-4'-thiocyano-p-toluenesulfonanilide

HRID 1356673

반응식

HRID 1356673 반응식
[S:1]([C:4]1[CH:20]=[CH:19][C:7]([NH:8][S:9]([C:12]2[CH:17]=[CH:16][C:15]([CH3:18])=[CH:14][CH:13]=2)(=[O:11])=[O:10])=[CH:6][CH:5]=1)[C:2]#[N:3].[N+:21]([O-])([OH:23])=[O:22].O>C(O)(=O)C>[N+:21]([C:6]1[CH:5]=[C:4]([S:1][C:2]#[N:3])[CH:20]=[CH:19][C:7]=1[NH:8][S:9]([C:12]1[CH:17]=[CH:16][C:15]([CH3:18])=[CH:14][CH:13]=1)(=[O:11])=[O:10])([O-:23])=[O:22]

참가 물질

5

반응물 3

HCID 944Nitric AcidHCID 962WaterHCID 8034834-{[(4-Methylphenyl)sulfonyl]amino}phenyl thiocyanate

생성물 1

HCID 185092522'-Nitro-4'-thiocyano-p-toluenesulfonanilide수율 99%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

4′-Thiocyano-p-toluenesulfonanilide (19.2 g (63.2 mmol)) was dissolved in acetic acid (60 ml). To this, fuming nitric acid (3.04 ml (75.9 mmol)) was added dropwise with stirring at room temperature. Then, the mixture was stirred at 50° C. for 4 hours, poured into water, and the crystals separated were filtered and washed with water. The resulting crystals were dissolved in ethyl acetate, and the solution was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure to give 21.8 g (99%) of 2′-nitro-4′-thiocyano-p-toluenesulfonanilide as pale yellow crystals.

후처리

  1. stirringThen, the mixture was stirred at 50° C. for 4 hours
  2. customthe crystals separated
  3. filtrationwere filtered
  4. washwashed with water
  5. dissolutionThe resulting crystals were dissolved in ethyl acetate
  6. dry with materialthe solution was dried over anhydrous magnesium sulfate
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-10eeae91fe154df3aab70945d8b1ac0a
출처 데이터셋
uspto-grants-2003_07
특허 번호
US06586617B1

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