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Hydrochloric Acid → WF 3681

HRID 1381372
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반응식

HRID 1381372 반응식
C(OC([O:6][C:7]1[C:11](=[O:12])[O:10][CH:9]([CH2:13][CH2:14][C:15]([OH:17])=[O:16])[C:8]=1[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)=O)C.C(=O)([O-])[O-].[K+].[K+].Cl>CO>[OH:6][C:7]1[C:11](=[O:12])[O:10][CH:9]([CH2:13][CH2:14][C:15]([OH:17])=[O:16])[C:8]=1[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 13389582HCID 13389582, 화합물

생성물 1

HCID 128356WF 3681수율 71%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

3-(4-Ethoxycarbonyloxy-5-oxo-3-phenyl-2,5-dihydro-2-furyl)propionic acid (20 mg) was dissolved in methanol (3 ml), and 10% aqueous potassium carbonate (3 ml) was added. The mixture was stirred at room temperature for 1 hour. The reaction mixture was poured into ice water (10 ml), acidified with hydrochloric acid, and extracted with ethyl acetate. The extract was washed with water and dried over magnesium sulfate. The solvent was then distilled off. The remaining oil was purified by preparative silice gel thin layer chromatography (developer: 5% methanol-chloroform). Recrystallization from chloroform gave 3-(4-hydroxy-5-oxo-3-phenyl-2,5-dihydro-2-furyl)propionic acid (11 mg) as colorless needles. m.p. 177°-179° C.

후처리

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with water
  3. dry with materialdried over magnesium sulfate
  4. distillationThe solvent was then distilled off
  5. customThe remaining oil was purified by preparative silice gel thin layer chromatography (developer: 5% methanol-chloroform)
  6. customRecrystallization from chloroform

출처 및 근거

ORD 기록
ord-8c10bd39fd584beba709a74aea824a17
출처 데이터셋
uspto-grants-1986_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04585789

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