Water → 2-[4'-(4"-Chlorophenoxy)phenoxy]-propionic acid 4-chlorobut-1-yl ester

HRID 903380ノート

反応式

HRID 903380 の反応式
[Cl:1][C:2]1[CH:20]=[CH:19][C:5]([O:6][C:7]2[CH:18]=[CH:17][C:10]([O:11][CH:12]([CH3:16])[C:13]([OH:15])=[O:14])=[CH:9][CH:8]=2)=[CH:4][CH:3]=1.[Cl:21][CH2:22][CH2:23][CH2:24][CH2:25]O.S(=O)(=O)(O)O.O>C(Cl)(Cl)Cl>[Cl:21][CH2:22][CH2:23][CH2:24][CH2:25][O:14][C:13](=[O:15])[CH:12]([O:11][C:10]1[CH:17]=[CH:18][C:7]([O:6][C:5]2[CH:4]=[CH:3][C:2]([Cl:1])=[CH:20][CH:19]=2)=[CH:8][CH:9]=1)[CH3:16]

参加物

6

反応物 4

HCID 962WaterHCID 1118Sulfuric AcidHCID 135694-Chloro-1-butanolHCID 64928Clofop

生成物 1

HCID 544272872-[4'-(4"-Chlorophenoxy)phenoxy]-propionic acid 4-chlorobut-1-yl ester

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

24.4 g=0.08 mol of 2-[4'-(4"-chlorophenoxy)phenoxy]-propionic acid, 10.8 g=0.1 mol of 4-chlorobutanol and 2 ml concentrated sulfuric acid in 50 ml chloroform were refluxed for 6 hours with azeotropic distillation of the reaction water. After cooling, the reaction mixture was washed twice with 100 ml water, neutralized with bicarbonate solution and washed with water until it was free from salt. After drying over calcium chloride and distillation of the solvent, 27.0 g=88% of the theory of 2-[4'-(4"-chlorophenoxy)phenoxy]-propionic acid 4-chlorobut-1-yl ester were obtained having a refractive index nD24 of 1.5517. ##STR16##

後処理

  1. temperatureAfter cooling
  2. washthe reaction mixture was washed twice with 100 ml water
  3. washwashed with water until it
  4. dry with materialAfter drying over calcium chloride and distillation of the solvent, 27.0 g=88% of the theory of 2-[4'-(4"-chlorophenoxy)phenoxy]-propionic acid 4-chlorobut-1-yl ester
  5. customwere obtained

出典と根拠

ORDレコード
ord-9eea7b03f4744be98d8b812d6cfd0338
出典データセット
uspto-grants-1980_10
特許番号
US04227009

反応ノート

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