Water → HCID 54488036, 화합물

HRID 1108768노트

반응식

HRID 1108768 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH:9]2[CH2:13][CH2:12][C:11](=O)[CH2:10]2)=[CH:5][CH:4]=1.[Cl-].[CH3:16][O:17][CH2:18][P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.CC(C)([O-])C.[K+].O>O1CCCC1.C(OCC)(=O)C>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH:9]2[CH2:13][CH2:12][C:11](=[CH:16][O:17][CH3:18])[CH2:10]2)=[CH:5][CH:4]=1

참가 물질

7

반응물 4

HCID 962WaterHCID 2723798Methoxymethyl-triphenylphosphonium chlorideHCID 140909103-(4-Methoxyphenyl)cyclopentan-1-oneHCID 23665647Potassium tert-butoxide

생성물 1

HCID 54488036HCID 54488036, 화합물수율 48.4%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

3-(4-Methoxyphenyl)cyclopentanone (8.51 g) and methoxymethyltriphenylphosphonium chloride (16.9 g) were dissolved in tetrahydrofuran (200 ml). After gradually adding potassium tert-butoxide (6.70 g) while maintaining an internal temperature of 10° C. or below, the mixture was stirred at room temperature for 2.5 hours. The reaction solution was poured into water, and extraction with ethyl acetate was followed by washing with water. After drying with anhydrous magnesium sulfate, the solvent was distilled off under reduced pressure to produce a brown oily substance which was then purified by silica gel column chromatography (n-hexane:ethyl acetate=20:1) to give 4.73 g of 1-methoxy-4-(3-methoxymethylenecyclopentyl) benzene (48.4% yield).

후처리

  1. washby washing with water
  2. dry with materialAfter drying with anhydrous magnesium sulfate
  3. distillationthe solvent was distilled off under reduced pressure
  4. customto produce a brown oily substance which
  5. customwas then purified by silica gel column chromatography (n-hexane:ethyl acetate=20:1)

출처 및 근거

ORD 기록
ord-781aa4627f2e42c38145a7a2825c7132
출처 데이터셋
uspto-grants-2000_05
특허 번호
US06069176

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