Hydrochloric Acid → HCID 18409104, 화합물

HRID 1586986노트

반응식

HRID 1586986 반응식
[CH3:1][NH:2][C:3]1([CH3:21])[CH2:12][CH2:11][CH2:10][C:9]2[N:8]=[C:7]([O:13]CC3C=CC=CC=3)[CH:6]=[CH:5][C:4]1=2.[ClH:22].[H][H]>C(O)C.CC(O)C.[Pd]>[ClH:22].[CH3:21][C:3]1([NH:2][CH3:1])[CH2:12][CH2:11][CH2:10][C:9]2[NH:8][C:7](=[O:13])[CH:6]=[CH:5][C:4]1=2

참가 물질

7

반응물 3

HCID 313Hydrochloric AcidHCID 18409092HCID 18409092, 화합물HCID 178418361HCID 178418361, 화합물2회

생성물 1

HCID 18409104HCID 18409104, 화합물수율 25%

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 702Ethanol용매HCID 3776Isopropanol용매

실험 절차

5,6,7,8-Tetrahydro-N,5-dimethyl-2-(phenylmethoxy)-5-quinolinamine (6.3 g) in ethanol (500 ml) was acidified to ca pH2 with a solution of hydrochloric acid in 2-propanol. 10% Palladium-on-carbon (315 mg) was added and the mixture was shaken on Parr hydrogenation apparatus, starting at 55 psi of hydrogen, until hydrogen uptake ceased. The catalyst was collected and the filtrate was neutralized with 4-polyvinylpyridine. The solution was concentrated in vacuo to a volume of about 75 ml and diethyl ether was added. The precipitate was collected and recrystallized first from methanol and then from water/2-propanol to afford 1.3 g (25%) of product, mp 190°-195° C. (dec).

후처리

  1. customThe catalyst was collected
  2. concentrationThe solution was concentrated in vacuo to a volume of about 75 ml and diethyl ether
  3. additionwas added
  4. customThe precipitate was collected
  5. customrecrystallized first from methanol

출처 및 근거

ORD 기록
ord-fb32d60553a34565882ce4bc40030d7e
출처 데이터셋
uspto-grants-1993_06
특허 번호
US05216164

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