Hydrochloric Acid → 4-(3-chlorophenyl)-1-ethyl-7-(1-hydroxyethyl)pyrido[2,3-d]pyrimidin-2(1H)-one

HRID 368990노트

반응식

HRID 368990 반응식
[OH-].[Na+].C([O:6][CH:7]([C:9]1[CH:10]=[CH:11][C:12]2[C:17]([C:18]3[CH:23]=[CH:22][CH:21]=[C:20]([Cl:24])[CH:19]=3)=[N:16][C:15](=[O:25])[N:14]([CH2:26][CH3:27])[C:13]=2[N:28]=1)[CH3:8])(=O)C.Cl>CO>[Cl:24][C:20]1[CH:19]=[C:18]([C:17]2[C:12]3[CH:11]=[CH:10][C:9]([CH:7]([OH:6])[CH3:8])=[N:28][C:13]=3[N:14]([CH2:26][CH3:27])[C:15](=[O:25])[N:16]=2)[CH:23]=[CH:22][CH:21]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 23284534HCID 23284534, 화합물

생성물 1

HCID 232844934-(3-chlorophenyl)-1-ethyl-7-(1-hydroxyethyl)pyrido[2,3-d]pyrimidin-2(1H)-one수율 75%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Methanol (30 ml) and 30 ml of 1 N sodium hydroxide aqueous solution were added to 6.78 g (18.2 mmol) of 7-(1-acetoxyethyl)-4-(3-chlorophenyl)-1-ethylpyrido[2,3-d]pyrimidin-2(1H)-one, followed by stirring for 20 minutes at room temperature. The reaction solution was neutralized by adding 1 N hydrochloric acid and extracted with chloroform. The organic layer was washed with brine and dried over anhydrous magnesium sulfate, magnesium sulfate was removed by filtration and the resulting filtrate was concentrated under a reduced pressure. Thereafter, the resulting residue was purified by silica gel column chromatography (chloroform) to give 4.50 g of 4-(3-chlorophenyl)-1-ethyl-7-(1-hydroxyethyl)pyrido[2,3-d]pyrimidin-2(1H)-one in the form of crystals. The yield was 75%.

후처리

  1. extractionextracted with chloroform
  2. washThe organic layer was washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate, magnesium sulfate
  4. customwas removed by filtration
  5. concentrationthe resulting filtrate was concentrated under a reduced pressure
  6. customThereafter, the resulting residue was purified by silica gel column chromatography (chloroform)

출처 및 근거

ORD 기록
ord-4d99e4ddd71d4555b5391b4d277b92fe
출처 데이터셋
uspto-grants-2000_10
특허 번호
US06136810

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