Malonic acid, disodium salt → Bicyclo[2,2,2]oct-5-ene-2-carbonyl malonic acid

HRID 1385850

反応式

HRID 1385850 の反応式
[C:1]([O-:7])(=[O:6])[CH2:2][C:3]([O-:5])=[O:4].[Na+].[Na+].[CH:10]12[CH2:17][CH2:16][CH:13]([CH:14]=[CH:15]1)[CH2:12][CH:11]2[C:18](Cl)=[O:19]>>[CH:10]12[CH2:17][CH2:16][CH:13]([CH:14]=[CH:15]1)[CH2:12][CH:11]2[C:18]([CH:2]([C:1]([OH:7])=[O:6])[C:3]([OH:5])=[O:4])=[O:19]

参加物

3

反応物 2

HCID 8865Malonic acid, disodium saltHCID 12935338Bicyclo[2,2,2]oct-5-ene-2-carbonyl chloride

生成物 1

HCID 22616776Bicyclo[2,2,2]oct-5-ene-2-carbonyl malonic acid収率 88%

実験手順

To a solution containing sodium malonate (17.1 g) which was prepared according to the same procedure as in Example 7, bicyclo[2,2,2]oct-5-ene-2-carbonyl chloride (17.1 g) obtained in Preparation Example 2 is slowly added, and the reaction mixture is reacted at −20° C. in a nitrogen atmosphere for 1 hour, and further reacted at 60° C. for 9 hours. Then, the mixture is worked up as in the procedure of Example 1, to obtain 21 g of the pure title compound (purity: 99%, yield: 88%).

後処理

  1. customwas prepared
  2. customobtained in Preparation Example 2
  3. additionis slowly added
  4. customthe reaction mixture is reacted at −20° C. in a nitrogen atmosphere for 1 hour
  5. customfurther reacted at 60° C. for 9 hours

出典と根拠

ORDレコード
ord-f02c3bd5bc6f455da78d8258dcadf398
出典データセット
uspto-grants-2001_07
特許番号
US06265130B1

関連ノート

読み込み中…