Hydrochloric Acid → HCID 18409104、化合物

HRID 1586986ノート

反応式

HRID 1586986 の反応式
[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

参加物

7

反応物 3

HCID 313Hydrochloric AcidHCID 18409092HCID 18409092、化合物HCID 178418361HCID 178418361、化合物2 回

生成物 1

HCID 18409104HCID 18409104、化合物収率 25%

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 702Ethanol溶媒HCID 3776Isopropanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-fb32d60553a34565882ce4bc40030d7e
出典データセット
uspto-grants-1993_06
特許番号
US05216164

反応ノート

読み込み中…