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Potassium Hydroxide → 1-(2',3'-Dimethyl-4'-methoxyphenoxy)-3-(tert.-butylamino)-2-propanol

HRID 2198859
ノート
印刷プレビュー

反応式

HRID 2198859 の反応式
[CH3:1][C:2]1[C:7]([CH3:8])=[C:6]([O:9][CH3:10])[CH:5]=[CH:4][C:3]=1[OH:11].[C:12]([N:16]1[CH2:19][CH:18]([OH:20])[CH2:17]1)([CH3:15])([CH3:14])[CH3:13].[OH-].[K+]>Cl>[CH3:1][C:2]1[C:7]([CH3:8])=[C:6]([O:9][CH3:10])[CH:5]=[CH:4][C:3]=1[O:11][CH2:17][CH:18]([OH:20])[CH2:19][NH:16][C:12]([CH3:13])([CH3:14])[CH3:15]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 14797Potassium HydroxideHCID 2879861-tert-Butyl-3-hydroxyazetidineHCID 109316254-Methoxy-2,3-dimethylphenol

生成物 1

HCID 130557041-(2',3'-Dimethyl-4'-methoxyphenoxy)-3-(tert.-butylamino)-2-propanol収率 72.5%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

反応条件

温度
140 °C

実験手順

A mixture of 9.1 parts of 2,3-dimethyl-4-methoxyphenol, 6.5 parts of 1-(tert.-butyl)-3-azetidinol and 0.3 part of potassium hydroxide was heated under nitrogen gas at 140° C. for 8 hours with agitation. The reaction product was dissolved in 100 parts of 2 N-hydrochloric acid aqueous solution and washed twice with 100 parts of ether. The water layer was made alkaline with 4 N-sodium hydroxide aqueous solution, and the resulting crystals were recovered by filtration and dried. Then the crystals were dissolved in 100 parts of ether and decolored. The decolored liquid was concentrated and allowed to cool. As a result, 10.2 parts of 1-(2',3'-dimethyl-4'-methoxyphenoxy)-3-(tert.-butylamino)-2-propanol melting at 73°-75° C. were obtained. The yield was 72.5%. The results of infra-red spectrum analysis and nuclear magnetic resonance analysis of the product are as follows:

後処理

  1. washwashed twice with 100 parts of ether
  2. filtrationthe resulting crystals were recovered by filtration
  3. customdried
  4. dissolutionThen the crystals were dissolved in 100 parts of ether
  5. concentrationThe decolored liquid was concentrated
  6. temperatureto cool

出典と根拠

ORDレコード
ord-de91f1af25ca4db8b7fe0ee53b575ded
出典データセット
uspto-grants-1982_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04360464

反応ノート

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