Hydrochloric Acid → 1-Chloro-5,5-dimethylnonan-4-one

HRID 1833772ノート

反応式

HRID 1833772 の反応式
[CH3:1][C:2]([Mg]Cl)([CH3:7])[CH2:3][CH2:4][CH2:5][CH3:6].[Mg].ClC(C)(C)CCCC.[Cl:19][CH2:20][CH2:21][CH2:22][C:23](Cl)=[O:24].Cl>CCOCC>[Cl:19][CH2:20][CH2:21][CH2:22][C:23](=[O:24])[C:2]([CH3:7])([CH3:1])[CH2:3][CH2:4][CH2:5][CH3:6]

参加物

7

実験手順

Four hundred ml. of a solution in ether of 1,1-dimethylpentylmagnesium chloride prepared from magnesium (24.3 g., 1.0 mole) and 1-chloro-1,1-dimethylpentane (134.5 g., 1.0 mole) according to the procedure of Whitmore and Badertscher [J. Am. Chem. Soc., 55, 1559 (1933)] is added dropwise with stirring to 4-chlorobutyryl chloride (197 g., 1.4 moles) in ether (400 ml.) during 6 hours. The reaction mixture is stirred for an additional 12 hours. It is then poured into a mixture of ice and dilute hydrochloric acid. The ether layer is separated, washed with water, and dried over sodium sulfate. The ether is evaporated and the residue distilled at aspirator vacuum through a Vigreaux column to yield the product as a colorless oil.

後処理

  1. additionis added dropwise
  2. customThe ether layer is separated
  3. washwashed with water
  4. dry with materialdried over sodium sulfate
  5. customThe ether is evaporated
  6. distillationthe residue distilled at aspirator vacuum through a Vigreaux column

出典と根拠

ORDレコード
ord-72325e0f24484262a67b034efcc0fde1
出典データセット
uspto-grants-1978_01
特許番号
US04066692

反応ノート

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