Malonic Acid → 3-Allyl-4-hydroxy-cinnamic acid
反応式
C(O[C:5]1[CH:6]=[C:7]([CH:10]=[CH:11][C:12]=1[OH:13])[CH:8]=O)C=C.[C:14]([OH:20])(=[O:19])[CH2:15]C(O)=O.N1CC[CH2:24][CH2:23][CH2:22]1>N1C=CC=CC=1>[CH2:24]([C:5]1[CH:6]=[C:7]([CH:10]=[CH:11][C:12]=1[OH:13])[CH:8]=[CH:15][C:14]([OH:20])=[O:19])[CH:23]=[CH2:22]参加物
5
実験手順
48.5 g (0.27 mol) of 3-allyloxy-4-hydroxy-benzaldehyde, 104 g (1 mol) of malonic acid, 140 ml of pyridine and 4 ml of piperidine are heated to 100° C for 2 hours, whilst stirring. The volatile constituents are distilled off under reduced pressure at 80° C and the residue is stirred with 800 ml of water. The crystals obtained are filtered off and recrystallised from methylene chloride. 3-Allyl-4-hydroxy-cinnamic acid of melting point 132°-133° C is obtained.
後処理
- distillationThe volatile constituents are distilled off under reduced pressure at 80° C
- stirringthe residue is stirred with 800 ml of water
- customThe crystals obtained
- filtrationare filtered off
- customrecrystallised from methylene chloride
出典と根拠
- ORDレコード
- ord-a06bdec0613d451da888b53ca52e0ae4
- 出典データセット
- uspto-grants-1977_03
- 特許番号
- US04014920
反応ノート
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