Ethanol → 4-(p-Fluorophenyl)-1,2,3,6-tetrahydro-1-[2-(p-nitrophenoxy)ethyl]pyridine

HRID 1605961ノート

反応式

HRID 1605961 の反応式
Cl.[F:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH2:10][CH2:11][NH:12][CH2:13][CH:14]=2)=[CH:5][CH:4]=1.Br[CH2:16][CH2:17][O:18][C:19]1[CH:24]=[CH:23][C:22]([N+:25]([O-:27])=[O:26])=[CH:21][CH:20]=1.C(=O)([O-])[O-].[K+].[K+].C(O)C>O>[F:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH2:14][CH2:13][N:12]([CH2:16][CH2:17][O:18][C:19]3[CH:20]=[CH:21][C:22]([N+:25]([O-:27])=[O:26])=[CH:23][CH:24]=3)[CH2:11][CH:10]=2)=[CH:5][CH:4]=1

参加物

6

反応物 4

HCID 702EthanolHCID 11430Potassium CarbonateHCID 1977474-(4-Fluorophenyl)-1,2,3,6-tetrahydropyridine hydrochlorideHCID 2359871-(2-Bromoethoxy)-4-nitrobenzene

生成物 1

HCID 215456084-(p-Fluorophenyl)-1,2,3,6-tetrahydro-1-[2-(p-nitrophenoxy)ethyl]pyridine

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 2.15 g. of 4-(p-fluorophenyl)-1,2,3,6-tetrahydropyridine hydrochloride, 2.5 g. of p-(2-bromoethoxy)-nitrobenzene, 2.8 g. of potassium carbonate, 20 ml. of ethanol and 2 ml. of water is refluxed for 3 days. After filtration the crude product crystallizes from the hot reaction mixture. It is purified by chromatography on silica gel using methylene chloride for elution. The 4-(p-fluorophenyl)-1,2,3,6-tetrahydro-1-[2-(p-nitrophenoxy)ethyl]pyridine obtained melts at 104°-107° after recrystallization from ethanol.

後処理

  1. additionA mixture of 2.15 g
  2. filtrationAfter filtration the crude product
  3. customcrystallizes from the hot reaction mixture
  4. customIt is purified by chromatography on silica gel
  5. washfor elution

出典と根拠

ORDレコード
ord-472af575e3384d15bb0fba58fced40f7
出典データセット
uspto-grants-1976_04
特許番号
US03951987

反応ノート

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