Malonic acid, disodium salt → Bicyclo[3,2,2]non-8-ene-2-carbonyl malonic acid

HRID 843189

反応式

HRID 843189 の反応式
[C:1]([O-:7])(=[O:6])[CH2:2][C:3]([O-:5])=[O:4].[Na+].[Na+].[CH:10]12[CH:18]=[CH:17][CH:14]([CH2:15][CH2:16]1)[CH2:13][CH2:12][CH:11]2[C:19](Cl)=[O:20]>>[CH:10]12[CH:16]=[CH:15][CH:14]([CH2:17][CH2:18]1)[CH2:13][CH2:12][CH:11]2[C:19]([CH:2]([C:1]([OH:7])=[O:6])[C:3]([OH:5])=[O:4])=[O:20]

参加物

3

反応物 2

HCID 8865Malonic acid, disodium saltHCID 22616798Bicyclo[3,2,2]non-8-ene-2-carbonyl chloride

生成物 1

HCID 22616774Bicyclo[3,2,2]non-8-ene-2-carbonyl malonic acid収率 87.5%

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[3,2,2]non-8-ene-2-carbonyl chloride (18.4 g) obtained in Preparation Example 3 is slowly added, and the reaction mixture is reacted at −20° C. in a nitrogen atmosphere for 1 hour, and further reacted at 45° C. for 8 hours. Then, the mixture is worked up as in the procedure of Example 1, to obtain 22 g of the pure title compound (purity: 99%, yield: 87%).

後処理

  1. customwas prepared
  2. customobtained in Preparation Example 3
  3. additionis slowly added
  4. customthe reaction mixture is reacted at −20° C. in a nitrogen atmosphere for 1 hour
  5. customfurther reacted at 45° C. for 8 hours

出典と根拠

ORDレコード
ord-551a1df4701a4d979ee8e42dd2d93ec2
出典データセット
uspto-grants-2002_04
特許番号
US06376632B1

関連ノート

読み込み中…