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

HRID 1905823

反応式

HRID 1905823 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-].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

7

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 2

HCID 3007855Zincchloride触媒HCID 962Water溶媒3 回

実験手順

To a solution of 34 parts of anhydrous zinc chloride in 51 parts of 36& w/w aqueous hydrochloric acid were added 46.5 parts of aniline and 18.2 parts of 6-hydroxy-6-methyl-2-heptylamine hydrochloride. The whole was charged to a 3-necked round bottomed flask fitted with a thermometer, stirrer, and Dean and Stark water separator. The stirred reaction mixture heated by means of an electric heating mantle was raised to a temperature of 185° C. by removal of water (Dean and Stark), and then maintained at this temperature for a further 18 hours. The hot reaction mixture was then poured slowly into a solution of 75 parts sodium hydroxide in 75 parts water and stirred until cool. The organic phase was extracted with ether, washed with water, evaporated and distilled under reduced pressure. After recovering 28 parts of aniline, there was obtained 18 parts of 2-amino-6-(4-aminophenyl)-6-methylheptane b12 192°-199° C. (82% yield based on heptaminol) with the following percentage composition by weight.

後処理

  1. additionThe whole was charged to a 3-necked round bottomed flask
  2. customThe stirred reaction mixture
  3. temperatureheated by means of an electric heating mantle
  4. temperaturemaintained at this temperature for a further 18 hours
  5. temperatureuntil cool
  6. extractionThe organic phase was extracted with ether
  7. washwashed with water
  8. customevaporated
  9. distillationdistilled under reduced pressure
  10. customAfter recovering 28 parts of aniline

出典と根拠

ORDレコード
ord-e0128aba3d9e43c8afd1451ba2df2749
出典データセット
uspto-grants-1987_03
特許番号
US04647699

関連ノート

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