Isobutyric anhydride → HCID 12851389、化合物

HRID 596981

反応式

HRID 596981 の反応式
[O:1]1[CH2:6][CH2:5][CH2:4]OO1.[C:7]([O:12][C:13](=[O:17])[CH:14]([CH3:16])[CH3:15])(=[O:11])C(C)C.Cl(O)(=O)(=O)=O.[C:23](=O)(O)[O-].[Na+]>>[C:13]([O:12][CH2:7][O:11][C:6](=[O:1])[CH:5]([CH3:23])[CH3:4])(=[O:17])[CH:14]([CH3:15])[CH3:16]

参加物

5

反応物 4

HCID 7346Isobutyric anhydrideHCID 24247Perchloric AcidHCID 516892Sodium BicarbonateHCID 19593658CID 19593658

生成物 1

HCID 12851389HCID 12851389、化合物

実験手順

A 30-g (0.33 mol) sample of trioxane was added to a solution of 158 g (1 mol) isobutyric anhydride and 0.5 ml 70% perchloric acid over a 30-minute period at 65°-70° C. The reaction mixture was then stirred until the temperature decreased to 27° C. The reaction mixture was diluted with saturated sodium bicarbonate solution and extracted with ether. The ether extracts were dried over magnesium sulfate and evaporated under reduced pressure. The resulting residue was distilled on a 30-cm column to give 112 g of methylene bisisobutyrate, b.p. 43°-48° C. at 0.2-0.3 mm of Hg and 30 g of oxybis-methylene isobutyrate, b.p. 57°-63° C. at 0.2-0.3 mm of Hg.

後処理

  1. customdecreased to 27° C
  2. extractionextracted with ether
  3. dry with materialThe ether extracts were dried over magnesium sulfate
  4. customevaporated under reduced pressure
  5. distillationThe resulting residue was distilled on a 30-cm column

出典と根拠

ORDレコード
ord-7156f543c297404f9f32044039980fb2
出典データセット
uspto-grants-1977_03
特許番号
US04012526

関連ノート

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