4-Pyridineacetic acid hydrochloride → HCID 18780247、化合物

HRID 345698

反応式

HRID 345698 の反応式
Cl.[N:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([OH:11])=[O:10])=[CH:4][CH:3]=1.[CH:12]([N:15]([CH:18]([CH3:20])[CH3:19])[CH2:16][CH3:17])(C)C>ClCCl>[CH3:12][N:15]1[C:18]2[C:20](=[CH:3][CH:4]=[CH:5][CH:19]=2)[C:17]([C:8]2[C:9](=[O:10])[O:10][C:9](=[O:11])[C:8]=2[C:5]2[CH:6]=[CH:7][N:2]=[CH:3][CH:4]=2)=[CH:16]1

参加物

4

反応物 2

HCID 810974-Pyridineacetic acid hydrochlorideHCID 81531Diisopropylethylamine2 回

生成物 1

HCID 18780247HCID 18780247、化合物収率 21.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

5 g of 4-pyridyl-acetic acid hydrochloride and 3.72 g of diisopropylethylamine in 50 ml of dichloromethane were treated at 0° C. firstly with 6.37 g of 1-methylindole-3-glyoxylyl chloride in 50 ml of dichloromethane and then with 7.5 g of diisopropylethylamine. The mixture was allowed to warm to room temperature and was then stirred for 65 hours. The solvent was removed under reduced pressure and the residue was taken up in dichloromethane and chromatographed on silica gel with ethyl acetate. The product-containing fractions were concentrated. Crystallization from ethyl acetate/hexane yielded 940 mg of 3-(1-methyl-3-indolyl)-4-(4-pyridyl)furan-2,5-dione, m.p. 217°-219° C.

後処理

  1. customThe solvent was removed under reduced pressure
  2. customchromatographed on silica gel with ethyl acetate
  3. concentrationThe product-containing fractions were concentrated
  4. customCrystallization from ethyl acetate/hexane

出典と根拠

ORDレコード
ord-cefa521c988b459f8532c75ce1a6145a
出典データセット
uspto-grants-1991_10
特許番号
US05057614

関連ノート

読み込み中…