Hydrochloric Acid → 2-[4-(4-Chlorophenoxy)-phenoxy]-propanol

HRID 263077ノート

反応式

HRID 263077 の反応式
[Cl:1][C:2]1[CH:20]=[CH:19][C:5]([O:6][C:7]2[CH:18]=[CH:17][C:10]([O:11][CH:12]([CH3:16])[C:13](O)=[O:14])=[CH:9][CH:8]=2)=[CH:4][CH:3]=1.[H-].[H-].[H-].[H-].[Li+].[Al+3].[H-].Cl>C(OCC)C.C(OCC)(=O)C>[Cl:1][C:2]1[CH:20]=[CH:19][C:5]([O:6][C:7]2[CH:18]=[CH:17][C:10]([O:11][CH:12]([CH3:16])[CH2:13][OH:14])=[CH:9][CH:8]=2)=[CH:4][CH:3]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 64928ClofopHCID 166653HydrideHCID 21226445Aluminium lithium hydride

生成物 1

HCID 128048842-[4-(4-Chlorophenoxy)-phenoxy]-propanol

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

A solution of 22.5 g (0.077 mol) of (±)-2-[4-(4-chlorophenoxy)-phenoxy]-propionic acid (CRL 40299) in 150 ml of anhydrous diethyl ether is run over the course of 1 hour 30 minutes into a suspension of 6.6 g (0.173 mol) of LiAlH4 in 50 ml of anhydrous diethyl ether. Thereafter the reflux is maintained for 1 hour 30 minutes, the excess hydride is neutralised with ethyl acetate and the complex is hydrolysed with dilute hydrochloric acid. The organic phase is decanted, washed with water and dilute sodium hydroxide solution and gives, after drying over dry sodium sulphate and evaporation of the solvent, 21.4 g of a crystalline white mass, which is insoluble in water.

後処理

  1. temperatureThereafter the reflux is maintained for 1 hour 30 minutes
  2. customThe organic phase is decanted
  3. washwashed with water and dilute sodium hydroxide solution
  4. customgives
  5. dry with materialafter drying over dry sodium sulphate and evaporation of the solvent, 21.4 g of a crystalline white mass, which

出典と根拠

ORDレコード
ord-5332fa105e0b48e7834e8392b8d3f779
出典データセット
uspto-grants-1979_05
特許番号
US04156011

反応ノート

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