Water → 4-Benzoyloxy-2,6-dichlorophenol

HRID 363090

반응식

HRID 363090 반응식
[C:1]([O:9][C:10]1[CH:15]=[CH:14][C:13]([OH:16])=C[CH:11]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Cl:17]OC(C)(C)C.O.[C:24]([Cl:28])(Cl)(Cl)Cl>>[C:1]([O:9][C:10]1[CH:15]=[C:14]([Cl:17])[C:13]([OH:16])=[C:24]([Cl:28])[CH:11]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 4

HCID 962WaterHCID 5943Carbon Tetrachloride2회HCID 75549p-Hydroxyphenyl benzoateHCID 521297Tert-Butyl hypochlorite

생성물 1

HCID 184293864-Benzoyloxy-2,6-dichlorophenol수율 91%

실험 절차

A reaction vessel was charged with 24.5 g of 4-hydroxyphenyl benzoate and 500 ml of carbon tetrachloride, to which a solution of 24.8 g of t-butyl hypochlorite dissolved in 20 ml of carbon tetrachloride was slowly added dropwise, while stirring under ice cooling. After 24 hours, the reaction mixture was poured into water, followed by phase separation. The organic layer (i.e., carbon tetrachloride layer) was washed with water, dried with anhydrous magnesium sulfate, and concentrated to obtain a crude product. The crude product was subjected to silica gel chromatography, which afforded 29.5 g of 3,5-dichloro-4-hydroxyphenyl benzoate (91% yield).

후처리

  1. additionwas slowly added dropwise
  2. customfollowed by phase separation
  3. washThe organic layer (i.e., carbon tetrachloride layer) was washed with water
  4. dry with materialdried with anhydrous magnesium sulfate
  5. concentrationconcentrated
  6. customto obtain a crude product

출처 및 근거

ORD 기록
ord-15d059fcbd8348ee972fd93d5e60d898
출처 데이터셋
uspto-grants-1999_02
특허 번호
US05872137

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