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Water → Ethyl 2-p-chlorophenyl-5-(2,5-dimethylphenoxy)-4-oxazoleacetate

HRID 46769
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HRID 46769 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[O:9][C:10]([O:17][C:18]3[CH:23]=[C:22]([CH3:24])[CH:21]=[CH:20][C:19]=3[CH3:25])=[C:11]([CH2:13][C:14]([OH:16])=[O:15])[N:12]=2)=[CH:4][CH:3]=1.[CH2:26](N(CC)CC)[CH3:27].C(Br)C.O>CN(C)C=O.C(OCC)(=O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[O:9][C:10]([O:17][C:18]3[CH:23]=[C:22]([CH3:24])[CH:21]=[CH:20][C:19]=3[CH3:25])=[C:11]([CH2:13][C:14]([O:16][CH2:26][CH3:27])=[O:15])[N:12]=2)=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 6332Ethyl BromideHCID 8471TriethylamineHCID 203856742-p-Chlorophenyl-5-(2,5-dimethylphenoxy)-4-oxazoleacetic acid

생성물 1

HCID 20385693Ethyl 2-p-chlorophenyl-5-(2,5-dimethylphenoxy)-4-oxazoleacetate

시약·촉매·용매 2

HCID 6228Dimethylformamide
용매
HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 0.80 g of 2-p-chlorophenyl-5-(2,5-dimethylphenoxy)-4-oxazoleacetic acid in 8 ml of dimethylformamide were added 1 ml of triethylamine and 1.5 ml of ethyl bromide. The mixture was stirred at 35°-40° C. for 90 minutes. The reaction mixture was poured into water and ethyl acetate and shaken with a separate funnel. The organic layer was successively washed with water, diluted hydrochloric acid and water, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The white crystalline residue was recrystallized from n-hexane to give 0.68 g of the title compound as white fine needles, melting at 122°-123.5° C.

후처리

  1. stirringshaken with a separate funnel
  2. washThe organic layer was successively washed with water, diluted hydrochloric acid and water
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe white crystalline residue was recrystallized from n-hexane

출처 및 근거

ORD 기록
ord-78d5fb0f79924ff3ba2378b92fb05498
출처 데이터셋
uspto-grants-1979_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04175130

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