Acetic Anhydride → Phenylitaconic anhydride

HRID 1109626

反応式

HRID 1109626 の反応式
C(OC(=O)C)(=O)C.[C:8]1(/[CH:14]=[C:15](\[CH2:19][C:20]([OH:22])=[O:21])/[C:16]([OH:18])=O)[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1>C1COCC1>[C:8]1([CH:14]=[C:15]2[CH2:19][C:20](=[O:21])[O:22][C:16]2=[O:18])[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1

参加物

4

反応物 2

HCID 7918Acetic AnhydrideHCID 820629(2E)-2-Benzylidenebutanedioic Acid

生成物 1

HCID 222996Phenylitaconic anhydride

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

2.3 l (approx. 2.49 kg, approx. 24.4 mol) of acetic anhydride are added at 20° C. to a solution of 2.28 kg (11.1 mol) of (E)-phenylitaconic acid in 5.7 l of THF. The mixture is stirred for 5 hours at room temperature. After 1 hour there is a clear light yellow solution; after 3 hours the product begins to crystallize out. The THF is removed under vacuum, 5.0 l of methyl tert-butyl ether are added to the residue in order to complete the crystallization, and the product is filtered off with suction. It is washed with MTB ether, dried with suction and dried under vacuum at 40° C. Yield: 1.68 kg (8.94 mol, 81% of theory), m.p. 167°-170° C.

後処理

  1. waitAfter 1 hour there is
  2. waitafter 3 hours the product begins
  3. customto crystallize out
  4. customThe THF is removed under vacuum, 5.0 l of methyl tert-butyl ether
  5. additionare added to the residue in order
  6. customthe crystallization
  7. filtrationthe product is filtered off with suction
  8. washIt is washed with MTB ether
  9. customdried with suction
  10. customdried under vacuum at 40° C

出典と根拠

ORDレコード
ord-893e78c5c79b454bb4ac749c2a386de9
出典データセット
uspto-grants-1994_06
特許番号
US05321139

関連ノート

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