Water → 4-Benzoyloxy-2,6-dichlorophenol

HRID 363090

反応式

HRID 363090 の反応式
[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

参加物

5

反応物 4

HCID 962WaterHCID 5943Carbon Tetrachloride2 回HCID 75549p-Hydroxyphenyl benzoateHCID 521297Tert-Butyl hypochlorite

生成物 1

HCID 184293864-Benzoyloxy-2,6-dichlorophenol収率 91%

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-15d059fcbd8348ee972fd93d5e60d898
出典データセット
uspto-grants-1999_02
特許番号
US05872137

関連ノート

読み込み中…