Sodium → Bicyclo[3,2,2]non-8-ene-2-carbonyl mono-tert-butyl malonate

HRID 1385849

반응식

HRID 1385849 반응식
[Na].[C:2]([O:8][C:9]([CH3:12])([CH3:11])[CH3:10])(=[O:7])[CH2:3][C:4]([O-:6])=[O:5].[CH:13]12[CH:21]=[CH:20][CH:17]([CH2:18][CH2:19]1)[CH2:16][CH2:15][CH:14]2[C:22](Cl)=[O:23]>>[C:4]([O:6][C:22]([CH:14]1[CH2:15][CH2:16][CH:17]2[CH:18]=[CH:19][CH:13]1[CH2:21][CH2:20]2)=[O:23])(=[O:5])[CH2:3][C:2]([O:8][C:9]([CH3:12])([CH3:11])[CH3:10])=[O:7]

참가 물질

4

반응물 3

HCID 5360545SodiumHCID 21883978Tert-butyl malonateHCID 22616798Bicyclo[3,2,2]non-8-ene-2-carbonyl chloride

생성물 1

HCID 86757166Bicyclo[3,2,2]non-8-ene-2-carbonyl mono-tert-butyl malonate수율 82%

실험 절차

To a solution of sodium salt of mono-tert-butyl malonate (20.4 g) prepared according to the same procedure as in Example 4, bicyclo[3,2,2]non-8-ene-2-carbonyl chloride (18.5 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 55° C. for 8 hours. Then, the mixture is worked up as in the procedure of Example 1, to obtain 25 g of the pure title compound (purity: 99%, yield: 82%).

후처리

  1. customobtained in Preparation Example 3
  2. additionis slowly added
  3. customthe reaction mixture is reacted at −20° C. in a nitrogen atmosphere for 1 hour
  4. customfurther reacted at 55° C. for 8 hours

출처 및 근거

ORD 기록
ord-aa08317f82c048889c5eb74ddf2b3732
출처 데이터셋
uspto-grants-2001_07
특허 번호
US06265130B1

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