Isopropanol → HCID 178517028、化合物

HRID 926517ノート

反応式

HRID 926517 の反応式
[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[NH:8][C:7](=[O:12])[CH:6]=[C:5]2[OH:13].[F:14][C:15]([F:25])([F:24])[C:16]1[CH:23]=[CH:22][C:19]([CH:20]=O)=[CH:18][N:17]=1.CC1NC(C)=C(C(OCC)=O)CC=1C(OCC)=O.C(O)(C)C>N1C=CC=CC=1>[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[C:7]([OH:12])[C:6]([CH2:20][C:19]1[CH:18]=[N:17][C:16]([C:15]([F:25])([F:14])[F:24])=[CH:23][CH:22]=1)=[C:5]2[OH:13]

参加物

6

実験手順

A mixture of 6-bromo-4-hydroxyquinolin-2(1H)-one (3.2 g, 18.3 mmol, Intermediate 45: step a), 6-(trifluoromethyl)nicotinaldehyde (4.0 g, 16.7 mmol) and diethyl 2,6-dimethyl-1,4-dihydropyridine-3,5-dicarboxylate (4.2 g, 16.7 mmol) in pyridine (34 mL) was heated to 105° C. for 3 hours. The solution was allowed to cool to ambient temperature, resulting in the formation of solid. Minimal isopropanol was added to the mixture and the slurry was stirred for 1 hour, sonicated, and filtered. The filtered solids were rinsed with isopropanol and dried under continuous air flow to provide the title compound as an off-white solid. Additional product was recrystallized from the filtrate, filtered, and rinsed with isopropanol.

後処理

  1. customresulting in the formation of solid
  2. customsonicated
  3. filtrationfiltered
  4. washThe filtered solids were rinsed with isopropanol
  5. customdried under continuous air flow

出典と根拠

ORDレコード
ord-20ab0f95149643e4afe75c18c2644d3c
出典データセット
uspto-grants-2016_03
特許番号
US09284308B2

反応ノート

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