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

HRID 1385851

반응식

HRID 1385851 반응식
[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]

참가 물질

3

반응물 2

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

생성물 1

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

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-39867a511f6d4a8a81a4a93ba40192ec
출처 데이터셋
uspto-grants-2001_07
특허 번호
US06265130B1

연결된 노트

불러오는 중…