Malonic Acid → 4-(Allyloxycarbonyl)benzoic acid

HRID 2268213ノート

反応式

HRID 2268213 の反応式
[CH:1]([C:3]1[CH:14]=[CH:13][C:6]([C:7]([O:9][CH2:10][CH:11]=[CH2:12])=[O:8])=[CH:5][CH:4]=1)=[O:2].C(O)(=O)CC(O)=[O:18].CCC1(CC)C(=O)NCCC1=O>N1C=CC=CC=1>[CH2:10]([O:9][C:7]([C:6]1[CH:13]=[CH:14][C:3]([C:1]([OH:18])=[O:2])=[CH:4][CH:5]=1)=[O:8])[CH:11]=[CH2:12]

参加物

5

反応物 3

HCID 867Malonic AcidHCID 64653,3-Diethyl-2,4-piperidinedioneHCID 18381245Allyl 4-formylbenzoate

生成物 1

HCID 183498554-(Allyloxycarbonyl)benzoic acid

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
100 °C

実験手順

17.2 g (90.5 mmol) of allyl 4-formylbenzoate, 24 g (230 mmol) of malonic acid, 8 ml of piperidione and 100 ml of pyridine are introduced into a round-bottomed flask. The reaction medium is heated at 100° C. for six hours and then evaporated to dryness. The residue is taken up in water and dichloromethane and acidified to pH 1, and the organic phase is separated out after settling has taken place, dried over magnesium sulphate and evaporated. The solid obtained is triturated from hexane, filtered off and dried. 16.7 g (80%) of 4-allyloxycarbonylbenzoic acid, with a melting point of 205-6° C., are collected.

後処理

  1. customevaporated to dryness
  2. customthe organic phase is separated out after settling
  3. dry with materialdried over magnesium sulphate
  4. customevaporated
  5. customThe solid obtained
  6. customis triturated from hexane
  7. filtrationfiltered off
  8. customdried
  9. custom16.7 g (80%) of 4-allyloxycarbonylbenzoic acid, with a melting point of 205-6° C., are collected

出典と根拠

ORDレコード
ord-95b2db39e87e42c7b1797e56b2fe9160
出典データセット
uspto-grants-2001_12
特許番号
US06326510B1

反応ノート

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