Hydrochloric Acid → HCID 610239、化合物

HRID 916501ノート

反応式

HRID 916501 の反応式
[C:1]([C:5]1[CH:12]=[CH:11][C:8]([CH:9]=O)=[CH:7][CH:6]=1)([O:3][CH3:4])=[O:2].[C:13]([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)(=[O:15])[CH3:14].C[O-].[Na+].Cl>CO.CCOC(C)=O>[CH3:4][O:3][C:1](=[O:2])[C:5]1[CH:12]=[CH:11][C:8]([CH:9]=[CH:14][C:13](=[O:15])[C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)=[CH:7][CH:6]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 7410AcetophenoneHCID 15294Methyl 4-FormylbenzoateHCID 10942334Sodium Methoxide

生成物 1

HCID 610239HCID 610239、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To 4-carbomethoxybenzaldehyde (79 mg, 0.48 mmol) and acetophenone (56 μL, 0.48 mmol) in anhydrous methanol (1.6 mL), was added neat sodium methoxide (26 mg, 0.48 mmol). The mixture was stirred at room temperature overnight then heated to reflux for 1 hour, cooled down to room temperature and added HCl 1N and EtOAc. The layers were separated and the organic layer dried over anhydrous MgSO4 and filtered. The solvent was evaporated under vacuum to afford a yellow solid, which was recrystallized from acetonitrile/water to give a pale yellow crystalline solid.

後処理

  1. temperaturethen heated
  2. temperatureto reflux for 1 hour
  3. temperaturecooled down to room temperature
  4. customThe layers were separated
  5. dry with materialthe organic layer dried over anhydrous MgSO4
  6. filtrationfiltered
  7. customThe solvent was evaporated under vacuum
  8. customto afford a yellow solid, which
  9. customwas recrystallized from acetonitrile/water
  10. customto give a pale yellow crystalline solid

出典と根拠

ORDレコード
ord-fc7e66cb4734493ebd68acb392428f13
出典データセット
uspto-grants-2007_09
特許番号
USRE039850E1

反応ノート

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