HCID 86676534, 화합물 → HCID 86676535, 화합물

HRID 73506노트

반응식

HRID 73506 반응식
[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

참가 물질

3

반응물 1

HCID 86676534HCID 86676534, 화합물

생성물 1

HCID 86676535HCID 86676535, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-cb04172a58b24eb7bf948b5f3270fa2a
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08829184B2

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