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

HRID 2397516ノート

反応式

HRID 2397516 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f3fb37cae190481695885369a90f55e4
出典データセット
uspto-grants-1977_05
特許番号
US04022672

反応ノート

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