Isopropanol → HCID 178517028, 화합물

HRID 926517노트

반응식

HRID 926517 반응식
[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]

참가 물질

6

반응물 4

HCID 3776IsopropanolHCID 70849Hantzsch esterHCID 27777626-(Trifluoromethyl)pyridine-3-carboxaldehydeHCID 546894466-Bromo-4-hydroxyquinolin-2(1H)-one

생성물 1

HCID 178517028HCID 178517028, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-20ab0f95149643e4afe75c18c2644d3c
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09284308B2

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