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

HRID 843187

反応式

HRID 843187 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[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]

参加物

4

反応物 3

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

生成物 1

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

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[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%).

後処理

  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

出典と根拠

ORDレコード
ord-9f53f1dcc4674301951e0ccffe8f8c7c
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…