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

HRID 1609662

반응식

HRID 1609662 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 223989604,5-Diacetoxy-2-pyridinecarbonyl chloride hydrochloride수율 158.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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 -2° 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).

후처리

  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

출처 및 근거

ORD 기록
ord-b412ab75ec36486d96b030f5dbc2df79
출처 데이터셋
uspto-grants-1995_03
특허 번호
US05401734

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