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Hydrochloric Acid → HCID 19004267、化合物

HRID 2225687
ノート
印刷プレビュー

反応式

HRID 2225687 の反応式
[Na+].[CH:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH:5]=[CH:4][C:3]=1[O:12][CH2:13][CH2:14][O:15][C:16]1[CH:21]=[CH:20][C:19]([C:22](=[O:26])[C:23]([O-:25])=[O:24])=[CH:18][CH:17]=1.Cl>ClCCl>[CH:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH:5]=[CH:4][C:3]=1[O:12][CH2:13][CH2:14][O:15][C:16]1[CH:21]=[CH:20][C:19]([C:22](=[O:26])[C:23]([OH:25])=[O:24])=[CH:18][CH:17]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 67756817HCID 67756817、化合物

生成物 1

HCID 19004267HCID 19004267、化合物収率 92.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 4-[[2-(2-naphthalenyloxy)ethyl]oxy]-alpha-oxobenzeneacetic acid sodium salt (3.0 g), dichloromethane (500 mL), and 1N hydrochloric acid (25 mL) was stirred for one hour until all solids dissolved. The layers were separated, the water layer was extracted 2×100 mL of dichloromethane and the organic layers were washed in turn with water. The combined organic layers were dried (Na2SO4), filtered and evaporated to give 2.8 g of crude product. Crystallization from dichloromethane-hexane provided 2.6 g of 4[[2- (2-naphthalenyloxy)ethyl]oxy]-alpha-oxobenzeneacetic acid, mp 170°-171° C.

後処理

  1. dissolutiondissolved
  2. customThe layers were separated
  3. extractionthe water layer was extracted 2×100 mL of dichloromethane
  4. washthe organic layers were washed in turn with water
  5. dry with materialThe combined organic layers were dried (Na2SO4)
  6. filtrationfiltered
  7. customevaporated
  8. customto give 2.8 g of crude product
  9. customCrystallization from dichloromethane-hexane

出典と根拠

ORDレコード
ord-bebf8df2aab747569b893325e7af4e7d
出典データセット
uspto-grants-1994_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05344843

反応ノート

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