Potassium Carbonate → HCID 19974504、化合物

HRID 1451658ノート

反応式

HRID 1451658 の反応式
Br[CH2:2][CH2:3][C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([N+:10]([O-:12])=[O:11])[CH:5]=1.Cl.[CH3:14][O:15][C:16]1[CH:17]=[C:18]2[C:23](=[CH:24][C:25]=1[O:26][CH3:27])[CH2:22][NH:21][CH2:20][CH2:19]2.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH3:14][O:15][C:16]1[CH:17]=[C:18]2[C:23](=[CH:24][C:25]=1[O:26][CH3:27])[CH2:22][N:21]([CH2:2][CH2:3][C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([N+:10]([O-:12])=[O:11])[CH:5]=1)[CH2:20][CH2:19]2

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 5916183-Nitrophenethyl bromideHCID 64560356,7-Dimethoxy-1,2,3,4-tetrahydroisoquinoline hydrochloride

生成物 1

HCID 19974504HCID 19974504、化合物収率 40.9%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 1-(2-bromoethyl)-3-nitrobenzene (2.3 g), 1,2,3,4-tetrahydro-6,7-dimethoxyisoquinoline hydrochloride (2.3 g) and potassium carbonate (3 g) in DMF (50 ml) was heated at 50° for 12 h. The mixture was then filtered and the filtrate evaporated. The residue was then taken up in water, extracted with dichloromethane, dried, evaporated and purified by column chromatography eluting with dichloromethane/methanol (99:1) to give the title compound (1.4 g) as a yellow oil. NMR includes signals at d 3.6 (2H,s,N--CH2Ar), 3.75 (6H,s,OCH3).

後処理

  1. temperaturewas heated at 50° for 12 h
  2. filtrationThe mixture was then filtered
  3. customthe filtrate evaporated
  4. extractionextracted with dichloromethane
  5. customdried
  6. customevaporated
  7. custompurified by column chromatography
  8. washeluting with dichloromethane/methanol (99:1)

出典と根拠

ORDレコード
ord-f7e030bc0b8d4cc5be3bf6e0961e3fba
出典データセット
uspto-grants-1997_02
特許番号
US05604237

反応ノート

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