Acetic Acid → Mls002703379

HRID 484784노트

반응식

HRID 484784 반응식
[C:1]1([CH3:19])[CH:6]=[CH:5][C:4]([S:7]([NH:10][C:11]2[C:16]([CH3:17])=[CH:15][CH:14]=[CH:13][C:12]=2[CH3:18])(=[O:9])=[O:8])=[CH:3][CH:2]=1.[N+:20]([O-])([OH:22])=[O:21].C(O)(=O)C.N([O-])=O.[Na+]>O>[C:1]1([CH3:19])[CH:2]=[CH:3][C:4]([S:7]([NH:10][C:11]2[C:16]([CH3:17])=[CH:15][C:14]([N+:20]([O-:22])=[O:21])=[CH:13][C:12]=2[CH3:18])(=[O:8])=[O:9])=[CH:5][CH:6]=1

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 944Nitric AcidHCID 262999N-(2,6-dimethylphenyl)-4-methylbenzenesulfonamideHCID 23668193Sodium Nitrite

생성물 1

HCID 263000Mls002703379

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

The sulfonamide intermediate of Example 4 (6.9 g, 0.025 mole) was added to a solution of 6.3 ml of concentrated nitric acid in 50 ml of water, followed by addition of 50 ml of glacial acetic acid and 0.18 g of sodium nitrite. The mixture was heated at reflux for one hour, then poured into 100 ml of water. The crude product thus isolated was recrystallized from ethanol to give 6.5 g of the title compound. Structure assignment was supported by the nmr spectrum and by elemental analysis.

후처리

  1. temperatureThe mixture was heated
  2. temperatureat reflux for one hour
  3. customThe crude product thus isolated
  4. customwas recrystallized from ethanol

출처 및 근거

ORD 기록
ord-608ef35de8e148e19da0a0f8ad804523
출처 데이터셋
uspto-grants-1985_08
특허 번호
US04533739

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