Ammonia → Tricyclo(5.2.1.0,2,6)decan-8-amine

HRID 2416992

반응식

HRID 2416992 반응식
[CH:1]12[CH2:11][CH:7]([C:8](=O)[CH2:9]1)[CH:6]1[CH:2]2[CH2:3][CH2:4][CH2:5]1.[NH3:12].[H][H]>CO.[Ni]>[CH2:3]1[CH:2]2[CH:6]([CH:7]3[CH2:11][CH:1]2[CH2:9][CH:8]3[NH2:12])[CH2:5][CH2:4]1

참가 물질

6

반응물 3

HCID 222AmmoniaHCID 965094,7-Methano-5H-inden-5-one, octahydro-HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 86760Tricyclo(5.2.1.0,2,6)decan-8-amine

시약·촉매·용매 2

HCID 935Nickel촉매HCID 887Methanol용매

실험 절차

A solution of 15 g of tricyclo[5,2,1,02,6]decan-8-one in 60 ml of methanol, which had been saturated beforehand at 10° C. with NH3, was, after addition of Raney nickel, hydrogenated in an autoclave at 90° C. and a hydrogen pressure of 100 bar for 10 hours. The catalyst was filtered off and the solvent was distilled off under reduced pressure, and the mixture was then made strongly alkaline using 10 N NaOH and extracted 2-3 times with ethyl acetate or with diisopropyl ether. The combined organic phases were dried and subjected to fractional distillation under reduced pressure. Bp6-7mm 86-88° C.

후처리

  1. customhydrogenated in an autoclave at 90° C.
  2. filtrationThe catalyst was filtered off
  3. distillationthe solvent was distilled off under reduced pressure
  4. extractionextracted 2-3 times with ethyl acetate
  5. customThe combined organic phases were dried
  6. distillationsubjected to fractional distillation under reduced pressure
  7. customBp6-7mm 86-88° C.

출처 및 근거

ORD 기록
ord-50cf7a5f055241dbbd55c2055c98f7b9
출처 데이터셋
uspto-grants-2004_11
특허 번호
US06825231B2

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