HCID 86676534、化合物 → HCID 86676535、化合物

HRID 73506ノート

反応式

HRID 73506 の反応式
[Cl:1][C:2]1[CH:27]=[CH:26][C:5]([CH2:6][O:7][C:8]2[CH:9]=[C:10]([CH:13]=[CH:14][C:15]=2[O:16]CC2C=CC(OC)=CC=2)[CH:11]=[O:12])=[CH:4][CH:3]=1>C(O)(=O)C>[Cl:1][C:2]1[CH:27]=[CH:26][C:5]([CH2:6][O:7][C:8]2[CH:9]=[C:10]([CH:13]=[CH:14][C:15]=2[OH:16])[CH:11]=[O:12])=[CH:4][CH:3]=1

参加物

3

反応物 1

HCID 86676534HCID 86676534、化合物

生成物 1

HCID 86676535HCID 86676535、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A solution of 3-(4-chloro-benzyloxy)-4-(4-methoxy-benzyloxy)-benzaldehyde (41)(108 g) in acetic acid (500 mL) was heated at reflux overnight. Excess acetic acid was removed by rotary evaporation under reduced pressure (hard vacuum) and the resulting residue taken up in ethyl acetate. The organic layer was extracted with aqueous sodium hydroxide solution (1 N; 3×150 mL). The combined inorganic phases were neutralised with conc. hydrochloric acid and back extracted with ethyl acetate. The organic layer was washed with brine and dried over magnesium sulphate. The resulting oil was triturated with 50/50 diethyl ether/hexane, the solid product 42 collected by vacuum filtration and the precipitate washed with hexane (32.6 g, 44%, retention time 3.08 mins, ES− 261.33).

後処理

  1. temperatureat reflux overnight
  2. customExcess acetic acid was removed by rotary evaporation under reduced pressure (hard vacuum)
  3. extractionThe organic layer was extracted with aqueous sodium hydroxide solution (1 N; 3×150 mL)
  4. extractionback extracted with ethyl acetate
  5. washThe organic layer was washed with brine
  6. dry with materialdried over magnesium sulphate
  7. customThe resulting oil was triturated with 50/50 diethyl ether/hexane
  8. filtrationthe solid product 42 collected by vacuum filtration
  9. washthe precipitate washed with hexane (32.6 g, 44%, retention time 3.08 mins, ES− 261.33)

出典と根拠

ORDレコード
ord-cb04172a58b24eb7bf948b5f3270fa2a
出典データセット
uspto-grants-2014_09
特許番号
US08829184B2

反応ノート

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