Water → HCID 54488036、化合物

HRID 1108768ノート

反応式

HRID 1108768 の反応式
[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

参加物

7

反応物 4

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

生成物 1

HCID 54488036HCID 54488036、化合物収率 48.4%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-781aa4627f2e42c38145a7a2825c7132
出典データセット
uspto-grants-2000_05
特許番号
US06069176

反応ノート

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