Sodium Hydroxide → 6-(4-chloro-2-pyridinyl)-2-pyridin-2-yl-1H-pyrimidin-4-one

HRID 721986

반응식

HRID 721986 반응식
C(O[C:4](=[O:15])[CH2:5][C:6]([C:8]1[CH:13]=[C:12]([Cl:14])[CH:11]=[CH:10][N:9]=1)=O)C.Cl.[C:17]([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][N:21]=1)(=[NH:19])[NH2:18].[OH-].[Na+]>C(O)C>[Cl:14][C:12]1[CH:11]=[CH:10][N:9]=[C:8]([C:6]2[N:19]=[C:17]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][N:21]=3)[N:18]=[C:4]([OH:15])[CH:5]=2)[CH:13]=1

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 12403615Pyridine-2-carboximidamide hydrochlorideHCID 534046173-(4-Chloropyrid-2-yl)-3-oxopropionic acid ethyl ester

생성물 1

HCID 1785156306-(4-chloro-2-pyridinyl)-2-pyridin-2-yl-1H-pyrimidin-4-one

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

13.15 g (58 mmol) of 3-(4-chloropyrid-2-yl)-3-oxopropionic acid ethyl ester are dissolved in 400 ml of ethanol, and 9.10 g (58 mmol) of 2-amidinopyridine hydrochloride are added. After the addition of 14.44 ml of 4N sodium hydroxide solution, refluxing is carried out for 7 hours. The mixture is cooled and concentrated to a fifth of its original volume. The crude product is filtered off and recrystallised from methanol, yielding 6-(4-chloropyrid-2-yl)-2-pyrid-2-yl-pyrimidin-4-ol in the form of beige needles.

후처리

  1. temperaturerefluxing
  2. temperatureThe mixture is cooled
  3. concentrationconcentrated to a fifth of its original volume
  4. filtrationThe crude product is filtered off
  5. customrecrystallised from methanol

출처 및 근거

ORD 기록
ord-0cff7a9880104f68a52f161de8ac4296
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07138363B2

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