Hydrochloric Acid → 5-(2,3-Dichloro-4-butyrylphenoxy)valeric acid

HRID 569260ノート

反応式

HRID 569260 の反応式
[Cl:1][C:2]1[C:7]([Cl:8])=[C:6]([C:9](=[O:13])[CH2:10][CH2:11][CH3:12])[CH:5]=[CH:4][C:3]=1[OH:14].C(=O)([O-])[O-].[K+].[K+].Br[CH2:22][CH2:23][CH2:24][CH2:25][C:26]([O:28]CC)=[O:27].[OH-].[Na+].Cl>CN(C)C=O.O>[Cl:1][C:2]1[C:7]([Cl:8])=[C:6]([C:9](=[O:13])[CH2:10][CH2:11][CH3:12])[CH:5]=[CH:4][C:3]=1[O:14][CH2:22][CH2:23][CH2:24][CH2:25][C:26]([OH:28])=[O:27]

参加物

8

反応物 5

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 14798Sodium HydroxideHCID 84580Ethyl 5-bromovalerateHCID 140998561-(2,3-Dichloro-4-hydroxyphenyl)butan-1-one

生成物 1

HCID 139587375-(2,3-Dichloro-4-butyrylphenoxy)valeric acid

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

A mixture of 2,3-dichloro-4-butyrylphenol (7 g, 0.03 mole), potassium carbonate (7.5 g, 0.054 mole) and ethyl 5-bromovalerate (9.5 g, 0.045 mole) in N,N-dimethylformamide (60 ml) were stirred and heated at 60° C. for 3 hours. The mixture was treated with 10 normal sodium hydroxide (12 ml) and water (50 ml), then stirred and heated on a steam bath for 2.5 hours. The solution was poured into ice water containing hydrochloric acid. The solid that separated was removed by filtration, washed with water and dried. The product (9.8 g) was recrystallized from butyl chloride to give 5-(2,3-dichloro-4-butyrylphenoxy)valeric acid, m.p. 102°-103° C.

後処理

  1. stirringstirred
  2. temperatureheated on a steam bath for 2.5 hours
  3. customThe solid that separated
  4. customwas removed by filtration
  5. washwashed with water
  6. customdried
  7. customThe product (9.8 g) was recrystallized from butyl chloride

出典と根拠

ORDレコード
ord-c8be41e1965d4e729271346f514fcdb7
出典データセット
uspto-grants-1988_03
特許番号
US04731473

反応ノート

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