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

HRID 1905823

반응식

HRID 1905823 반응식
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]

참가 물질

7

반응물 4

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

생성물 1

HCID 201566692-Amino-6-(4-aminophenyl)-6-methylheptane수율 82%

시약·촉매·용매 2

HCID 3007855Zincchloride촉매HCID 962Water용매3회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e0128aba3d9e43c8afd1451ba2df2749
출처 데이터셋
uspto-grants-1987_03
특허 번호
US04647699

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