Methanol → 2(3H)-Furanone, 5-(2,2-dichloroethenyl)dihydro-4,4-dimethyl-

HRID 358538ノート

反応式

HRID 358538 の反応式
[OH-].[Na+].O.CO.[CH3:6][C:7]([CH3:21])([CH:14](Cl)[CH2:15][C:16](Cl)([Cl:18])[Cl:17])[CH2:8][C:9]([O:11]CC)=[O:10]>CCOCC>[CH3:6][C:7]1([CH3:21])[CH:14]([CH:15]=[C:16]([Cl:18])[Cl:17])[O:11][C:9](=[O:10])[CH2:8]1

参加物

6

反応物 4

HCID 887MethanolHCID 962WaterHCID 14798Sodium HydroxideHCID 108412Hexanoic acid, 4,6,6,6-tetrachloro-3,3-dimethyl-, ethyl ester

生成物 1

HCID 101982032(3H)-Furanone, 5-(2,2-dichloroethenyl)dihydro-4,4-dimethyl-収率 92%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

To a mixed solution of 12.0 parts of sodium hydroxide, 40 parts of water and 60 parts of methanol was added dropwise under reflux 31.0 parts of ethyl 3,3-dimethyl-4,6,6,6-tetrachlorohexanoate and, after the dropwise addition had been completed, the mixture was stirred at that temperature for 2 hours. The reaction mixture was then distilled under reduced pressure to remove the methanol, and the residue was neutralized with hydrochloric acid and extracted with diethyl ether. From this ether layer was obtained 19.2 parts of 3,3-dimethyl-4-(2',2'-dichlorovinyl)-4-butanolide (yield 92%) which had the following properties.

後処理

  1. additionafter the dropwise addition
  2. distillationThe reaction mixture was then distilled under reduced pressure
  3. customto remove the methanol
  4. extractionextracted with diethyl ether

出典と根拠

ORDレコード
ord-fd5ae1c67d814119ba0c2a48c1d73e56
出典データセット
uspto-grants-1984_08
特許番号
US04468521

反応ノート

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