Sodium → Bicyclo[2,2,2]oct-5-ene-2-carbonyl mono-tert-butyl malonate

HRID 843186

反応式

HRID 843186 の反応式
[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[CH2:20][CH2:19][CH:16]([CH:17]=[CH:18]1)[CH2:15][CH:14]2[C:21](Cl)=[O:22]>>[C:4]([O:6][C:21]([CH:14]1[CH2:15][CH:16]2[CH2:19][CH2:20][CH:13]1[CH:18]=[CH:17]2)=[O:22])(=[O:5])[CH2:3][C:2]([O:8][C:9]([CH3:12])([CH3:11])[CH3:10])=[O:7]

参加物

4

反応物 3

HCID 5360545SodiumHCID 12935338Bicyclo[2,2,2]oct-5-ene-2-carbonyl chlorideHCID 21883978Tert-butyl malonate

生成物 1

HCID 86757165Bicyclo[2,2,2]oct-5-ene-2-carbonyl mono-tert-butyl malonate収率 84.8%

実験手順

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[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 40° C. for 6 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: 84%).

後処理

  1. customobtained in Preparation Example 2
  2. additionis slowly added
  3. customthe reaction mixture is reacted at −20° C. in a nitrogen atmosphere for 1 hour
  4. customfurther reacted at 40° C. for 6 hours

出典と根拠

ORDレコード
ord-dd1fbf0d7f0e40c196e3a024637f9766
出典データセット
uspto-grants-2002_04
特許番号
US06376632B1

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