4-Pyridineacetic acid hydrochloride → HCID 18780247, 화합물

HRID 345698

반응식

HRID 345698 반응식
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

참가 물질

4

반응물 2

HCID 810974-Pyridineacetic acid hydrochlorideHCID 81531Diisopropylethylamine2회

생성물 1

HCID 18780247HCID 18780247, 화합물수율 21.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-cefa521c988b459f8532c75ce1a6145a
출처 데이터셋
uspto-grants-1991_10
특허 번호
US05057614

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