Hydrochloric Acid → 2-Amino-6-(4-aminophenyl)-6-methylheptane

HRID 2296370

反応式

HRID 2296370 の反応式
Cl.[NH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.Cl.O[C:11]([CH3:19])([CH3:18])[CH2:12][CH2:13][CH2:14][CH:15]([NH2:17])[CH3:16].[OH-].[Na+]>[Cl-].[Zn+2].[Cl-].[Ta].O>[NH2:17][CH:15]([CH2:14][CH2:13][CH2:12][C:11]([C:6]1[CH:7]=[CH:8][C:3]([NH2:2])=[CH:4][CH:5]=1)([CH3:19])[CH3:18])[CH3:16]

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 6115AnilineHCID 10969Heptaminol HydrochlorideHCID 14798Sodium Hydroxide

生成物 1

HCID 201566692-Amino-6-(4-aminophenyl)-6-methylheptane収率 82%

試薬・触媒・溶媒 3

HCID 23956Tantalum触媒HCID 3007855Zincchloride触媒HCID 962Water溶媒2 回

反応条件

温度
185 °C

実験手順

To a solution of 102 parts of anhydrous zinc chloride in 153 parts of 36% w/w aqueous hydrochloric acid and 200 parts of water are added 140 parts of aniline and 136 parts of 6-hydroxy-6-methyl-2-heptylamine hydrochloride (heptaminol hydrochloride). The whole is charged to a 1 liter tantalum-lined autoclave and stirred at 185° C. for 24 hours. The reaction mixture, after being discharged from the autoclave, is added to a hot solution of 750 parts sodium hydroxide in 1500 parts of water and stirred until cool. The organic phase is extracted with diethylether, washed with water, evaporated and distilled under reduced pressure. After recovering 58 parts of aniline there are obtained 135 parts of 2-amino-6-(4-amino-phenyl)-6-methyl-heptane boiling point 138°-40° C./65 Pa (82% yield based on heptaminol).

後処理

  1. stirringstirred
  2. temperatureuntil cool
  3. extractionThe organic phase is extracted with diethylether
  4. washwashed with water
  5. customevaporated
  6. distillationdistilled under reduced pressure
  7. customAfter recovering 58 parts of aniline

出典と根拠

ORDレコード
ord-3e401ff2a45b426fa5a1c001b420fd1b
出典データセット
uspto-grants-1984_01
特許番号
US04429110

関連ノート

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