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

HRID 569260노트

반응식

HRID 569260 반응식
[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]

참가 물질

8

반응물 5

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

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온도
60 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c8be41e1965d4e729271346f514fcdb7
출처 데이터셋
uspto-grants-1988_03
특허 번호
US04731473

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