Hydrochloric Acid → 4-Ethoxycinnamic Acid

HRID 517578

反応式

HRID 517578 の反応式
[CH2:1]([O:3][C:4]1[CH:11]=[CH:10][C:7]([CH:8]=O)=[CH:6][CH:5]=1)[CH3:2].N1CCCCC1.C(O)(=O)[CH2:19][C:20]([OH:22])=[O:21].Cl>N1C=CC=CC=1>[CH2:1]([O:3][C:4]1[CH:11]=[CH:10][C:7](/[CH:8]=[CH:19]/[C:20]([OH:22])=[O:21])=[CH:6][CH:5]=1)[CH3:2]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 867Malonic AcidHCID 8082PiperidineHCID 248344-Ethoxybenzaldehyde

生成物 1

HCID 7042184-Ethoxycinnamic Acid

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒2 回

反応条件

温度
120 °C

実験手順

A solution of 4-ethoxybenzaldehyde (1.00 mL, 7.20 mmol) and piperidine (0.11 mL, 1.08 mmol) in 40 mL of pyridine was heated to 120° C. A solution of malonic acid (1.50 g, 14.40 mmol) in 40 mL of pyridine was added dropwise over 30 min and the reaction solution was stirred at 120° C. for 4 h. After cooling down to 0° C., excess amount of concentrated HCl was added carefully to make ˜pH 1. A white crystalline precipitate formed, and the solid was collected by filtration, washed with 0.1 N HCl aqueous solution, and dried to afford compound 19 in 99.5% (1.40 g) of pure 19 as a white solid.

後処理

  1. temperatureAfter cooling down to 0° C.
  2. customA white crystalline precipitate formed
  3. filtrationthe solid was collected by filtration
  4. washwashed with 0.1 N HCl aqueous solution
  5. customdried

出典と根拠

ORDレコード
ord-e34d4247259b419bbe12ceed44badcf1
出典データセット
uspto-grants-2015_08
特許番号
US09115122B2

関連ノート

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