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Water → HCID 10398790、化合物

HRID 654686
ノート
印刷プレビュー

反応式

HRID 654686 の反応式
O[C:2]([C:5]1[CH:6]=[CH:7][CH:8]=[C:9]2[C:14]=1[C:13]([OH:15])=[CH:12][CH:11]=[CH:10]2)([CH3:4])[CH3:3].[OH2:16].N1[CH:22]=[CH:21]C=CC=1>C(O)(=O)C>[C:21]([O:15][C:13]1[C:14]2[C:9](=[CH:8][CH:7]=[CH:6][C:5]=2[C:2]([CH3:4])=[CH2:3])[CH:10]=[CH:11][CH:12]=1)(=[O:16])[CH3:22]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 1049PyridineHCID 10262250HCID 10262250、化合物

生成物 1

HCID 10398790HCID 10398790、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
60 °C

実験手順

11.3 g of 8-(1-hydroxy-1-methyl-1-ethyl)-1-naphthol was dissolved in 24 ml of pyridine, to which 12 ml of anhydrous acetic acid was added. The solution was raised in temperature to 60° C. and heated for 6 hours under agitation. Water was added to the reaction solution, followed by extraction with ethyl acetate. The resulting organic phase was washed with a 2N hydrochloric acid aqueous solution, water and a saturated saline solution in this order, dried with anhydrous magnesium sulfate, and concentrated under reduced pressure. The resultant residue was purified by silica gel column chromatography (10% ethyl acetate/hexane) to obtain 3.6 g of the captioned compound as an oily substance.

後処理

  1. additionwas added
  2. temperatureheated for 6 hours under agitation
  3. extractionfollowed by extraction with ethyl acetate
  4. washThe resulting organic phase was washed with a 2N hydrochloric acid aqueous solution, water
  5. dry with materiala saturated saline solution in this order, dried with anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe resultant residue was purified by silica gel column chromatography (10% ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-10504e77714048f58ef71225b6bcbfc3
出典データセット
uspto-grants-1992_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05134111

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート