Pyridine → 1,1,1-Trichloro-2-acetoxy-4-methyl-3-pentene

HRID 2397516노트

반응식

HRID 2397516 반응식
[Cl:1][C:2]([Cl:10])([Cl:9])[CH:3]([OH:8])[CH:4]=[C:5]([CH3:7])[CH3:6].[C:11](OC(=O)C)(=[O:13])[CH3:12].N1C=CC=CC=1>CCCCCC>[Cl:1][C:2]([Cl:10])([Cl:9])[CH:3]([O:8][C:11](=[O:13])[CH3:12])[CH:4]=[C:5]([CH3:7])[CH3:6]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 7918Acetic AnhydrideHCID 30144241,1,1-Trichloro-4-methylpent-3-en-2-ol

생성물 1

HCID 127427841,1,1-Trichloro-2-acetoxy-4-methyl-3-pentene수율 81.3%

시약·촉매·용매 1

HCID 8058Hexane용매

실험 절차

A mixture of 53 g of 1,1,1-trichloro-2-hydroxy-4-methyl-3-pentene, 28 g of acetic anhydride, and 1.23 ml of pyridine was heated at 95°-100° for one hour. The reaction mixture was then dissolved in 500 ml of hexane. This solution was washed thrice with 150 ml portions of water and dried over anhydrous magnesium sulfate. After stripping the hexane, the residue was distilled under reduced pressure, yielding 52 g of 1,1,1-trichloro-2-acetoxy-4-methyl-3-pentene; bp 85°-90°/4-4.3 mm. An nmr spectrum of this product was consistent with the assigned structure.

후처리

  1. temperaturewas heated at 95°-100° for one hour
  2. washThis solution was washed thrice with 150 ml portions of water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationthe residue was distilled under reduced pressure

출처 및 근거

ORD 기록
ord-f3fb37cae190481695885369a90f55e4
출처 데이터셋
uspto-grants-1977_05
특허 번호
US04022672

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