Pyridine → 2-Chloro-alpha-phenyl-3-pyridinemethanol monophthalate

HRID 648724

反応式

HRID 648724 の反応式
[C:1]1(=[O:11])[O:6][C:4](=[O:5])[C:3]2=[CH:7][CH:8]=[CH:9][CH:10]=[C:2]12.[Cl:12][C:13]1[C:18]([CH:19]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[OH:20])=[CH:17][CH:16]=[CH:15][N:14]=1.N1C=CC=CC=1>CCOCC>[C:1]([OH:6])(=[O:11])[C:2]1[C:3](=[CH:7][CH:8]=[CH:9][CH:10]=1)[C:4]([OH:20])=[O:5].[Cl:12][C:13]1[C:18]([CH:19]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[OH:20])=[CH:17][CH:16]=[CH:15][N:14]=1

参加物

5

反応物 3

HCID 1049PyridineHCID 6811Phthalic AnhydrideHCID 30619803-Pyridinemethanol, 2-chloro-alpha-phenyl-

生成物 1

HCID 867410462-Chloro-alpha-phenyl-3-pyridinemethanol monophthalate収率 113.9%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

0.37 g phthalic anhydride, 0.50 g 2-chloro-α-phenyl-3-pyridinemethanol and 3 ml pyridine are heated at 100° C. for 7 hrs. The reaction mixture is diluted with ether and extracted twice with aqueous sodium carbonate. The aqueous extracts, after washing with ether, are acidified with 2N HCl, affording 0.5 g title product, m.p. 173°-4° C. (ethanol:water); neutralization equivalent: 372 (calculated 367.8); Cl 9.73 (9.64).

後処理

  1. extractionextracted twice with aqueous sodium carbonate
  2. washThe aqueous extracts, after washing with ether

出典と根拠

ORDレコード
ord-65ced4ed1fd64161adcc76da2475011b
出典データセット
uspto-grants-1988_04
特許番号
US04736037

関連ノート

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