Sulfuric Acid → HCID 9903943, 화합물

HRID 2304075노트

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HRID 2304075 반응식
[C:1]([C:3]1[C:11]([Cl:12])=[C:10]([Cl:13])[C:6]([C:7](N)=[O:8])=[C:5]([Cl:14])[C:4]=1[Cl:15])#[N:2].Cl[O-].[Na+].S(=O)(=O)(O)[OH:20]>O>[C:1]([C:3]1[C:11]([Cl:12])=[C:10]([Cl:13])[C:6]([C:7]([OH:20])=[O:8])=[C:5]([Cl:14])[C:4]=1[Cl:15])#[N:2]

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 9925815HCID 9925815, 화합물HCID 23665760Sodium Hypochlorite

생성물 1

HCID 9903943HCID 9903943, 화합물수율 92%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
15 °C

실험 절차

4-Cyano-2,3,5,6-tetrachlorobenzamide (284 g) which had been synthesized separately and water (2556 g) were placed in a four-neck flask, and the mixture was cooled to 15° C. with stirring. Subsequently, an aqueous solution (2360 g) of sodium hypochlorite (effective chlorine 12%) was added to the reaction mixture over six hours while a 50% aqueous solution of sulfuric acid was added so as to maintain the pH of the mixture at 5-6. Liquid chromatographic analysis revealed that the reaction mixture contained 262.2 g of 4-cyano-2,3,5,6-tetrachlorobenzoic acid (yield 92%).

후처리

  1. additionwas added so as
  2. temperatureto maintain the pH of the mixture at 5-6

출처 및 근거

ORD 기록
ord-518d01e404cf401ab46ac1c0b037c3e1
출처 데이터셋
uspto-grants-2002_08
특허 번호
US06433211B1

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