Acetic Anhydride → 1,1-Cyclohexanediacetic Anhydride

HRID 227340

反応式

HRID 227340 の反応式
[C:1]1([CH2:11][C:12]([OH:14])=[O:13])([CH2:7][C:8]([OH:10])=O)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C(OC(=O)C)(=O)C>>[C:1]12([CH2:7][C:8](=[O:10])[O:14][C:12](=[O:13])[CH2:11]1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]2

参加物

3

反応物 2

HCID 7918Acetic AnhydrideHCID 78061Cyclohexanediacetic acid

生成物 1

HCID 27342891,1-Cyclohexanediacetic Anhydride収率 100%

実験手順

A suspension of 1,1-cyclohexanediacetic acid (39.95 mmol) in acetic anhydride (159.8 mmol) was refluxed gently until a clear solution was obtained (ca. 1 h). The reaction mixture was kept at reflux for another hour until the reaction was complete. The reaction mixture was cooled to room temperature and acetic acid and excess acetic anhydride were removed under vacuum to afford 7.28 g (100%) of (3). 1H NMR (CDCl3): 2.65 (4H, s); 1.54-1.43 (10H, m).

後処理

  1. temperaturewas refluxed gently until a clear solution
  2. customwas obtained (ca. 1 h)
  3. temperatureat reflux for another hour until the reaction
  4. customacetic acid and excess acetic anhydride were removed under vacuum

出典と根拠

ORDレコード
ord-2b67861576314e4ebf8b42096805df53
出典データセット
uspto-grants-2009_07
特許番号
US07560483B2

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