Diisopropyl Ether → 4,5-Diacetoxy-2-pyridinecarbonyl chloride hydrochloride

HRID 5520

反応式

HRID 5520 の反応式
P(Cl)(Cl)(Cl)(Cl)[Cl:2].[C:7]([O:10][C:11]1[C:16]([O:17][C:18](=[O:20])[CH3:19])=[CH:15][N:14]=[C:13]([C:21]([OH:23])=O)[CH:12]=1)(=[O:9])[CH3:8].C(OC(C)C)(C)C>C(Cl)Cl>[ClH:2].[C:7]([O:10][C:11]1[C:16]([O:17][C:18](=[O:20])[CH3:19])=[CH:15][N:14]=[C:13]([C:21]([Cl:2])=[O:23])[CH:12]=1)(=[O:9])[CH3:8]

参加物

5

反応物 3

HCID 7914Diisopropyl EtherHCID 24819Phosphorus pentachlorideHCID 150773054,5-Diacetoxy-2-pyridinecarboxylic acid

生成物 1

HCID 223989604,5-Diacetoxy-2-pyridinecarbonyl chloride hydrochloride収率 158.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a suspension of phosphorus pentachloride (4.6 g) in methylene chloride (40 ml) was added 4,5-diacetoxy-2-pyridinecarboxylic acid (4.5 g) at -20° C. with stirring. The stirring was continued for an hour at -18°~12° C. To the reaction mixture was added diisopropyl ether (80 ml) below 0° C. The resulting precipitates were collected by filtration, washed with diisopropyl ether and dried over phosphorus pentoxide to give 4,5-diacetoxy-2-pyridinecarbonyl chloride hydrochloride (5.15 g).

後処理

  1. waitThe stirring was continued for an hour at -18°~12° C
  2. customThe resulting precipitates
  3. filtrationwere collected by filtration
  4. washwashed with diisopropyl ether
  5. dry with materialdried over phosphorus pentoxide

出典と根拠

ORDレコード
ord-2ef62d98fe1447439390fdc1af915ab7
出典データセット
uspto-grants-1993_09
特許番号
US05244890

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