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

HRID 2296370

반응식

HRID 2296370 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-].[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]

참가 물질

8

반응물 4

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

생성물 1

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

시약·촉매·용매 3

HCID 23956Tantalum촉매HCID 3007855Zincchloride촉매HCID 962Water용매2회

반응 조건

온도
185 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-3e401ff2a45b426fa5a1c001b420fd1b
출처 데이터셋
uspto-grants-1984_01
특허 번호
US04429110

연결된 노트

불러오는 중…