Sodium Carbonate → 2-Chloro-3-octyl-6-(4-octyloxyphenyl)pyridine

HRID 1780544ノート

反応式

HRID 1780544 の反応式
[CH2:1]([C:9]1[C:10](=O)[NH:11][C:12]([C:15]2[CH:20]=[CH:19][C:18]([O:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH3:29])=[CH:17][CH:16]=2)=[CH:13][CH:14]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].O=P(Cl)(Cl)[Cl:33].C(=O)([O-])[O-].[Na+].[Na+]>>[Cl:33][C:10]1[C:9]([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8])=[CH:14][CH:13]=[C:12]([C:15]2[CH:20]=[CH:19][C:18]([O:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH3:29])=[CH:17][CH:16]=2)[N:11]=1

参加物

4

反応物 3

HCID 10340Sodium CarbonateHCID 24813Phosphorus oxychlorideHCID 190469563-octyl-6-(4-octyloxyphenyl)-1H-2-pyridone

生成物 1

HCID 190469532-Chloro-3-octyl-6-(4-octyloxyphenyl)pyridine

実験手順

0.32 g (0.8 mmol) of 3-octyl-6-(4-octyloxyphenyl)-1H-2-pyridone are heated together with 15 ml of phosphorus oxytrichloride in a sealed tube at 200° C. for 3 hours. The reaction mixture is poured onto ice water, and the resulting mixture is made basic with sodium carbonate. Extraction of the aqueous phase with methylene chloride, washing of the organic phase with sodium chloride solution, drying over sodium sulfate, filtration, removal of the solvent by distillation and chromatography (silica gel, 8:2 hexane/ethyl acetate) give 0.22 g of 2-chloro-3-octyl-6-(4-octyloxyphenyl)pyridine. ##STR15##

後処理

  1. additionThe reaction mixture is poured onto ice water
  2. extractionExtraction of the aqueous phase with methylene chloride
  3. washwashing of the organic phase with sodium chloride solution
  4. dry with materialdrying over sodium sulfate, filtration, removal of the solvent by distillation and chromatography (silica gel, 8:2 hexane/ethyl acetate)

出典と根拠

ORDレコード
ord-976049ba478e4e3795c005d854371c91
出典データセット
uspto-grants-1997_05
特許番号
US05630962

反応ノート

読み込み中…