Water → 5-phenyl-1H-pyrazin-2-one

HRID 1747776

반응식

HRID 1747776 반응식
Cl.[NH2:2][CH2:3][C:4]([NH2:6])=[O:5].O.[OH-].[Na+].O=[C:11]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[CH:12]=O>CO.C(O)(=O)C>[C:14]1([C:11]2[N:2]=[CH:3][C:4](=[O:5])[NH:6][CH:12]=2)[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1

참가 물질

7

반응물 4

HCID 962WaterHCID 14090PhenylglyoxalHCID 14798Sodium Hydroxide2회HCID 2723639Glycinamide hydrochloride

생성물 1

HCID 5990375-phenyl-1H-pyrazin-2-one수율 75.6%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 887Methanol용매3회

반응 조건

온도
-20 °C

실험 절차

To a mixture of glycine amide hydrochloride (0.73 g), methanol (6.0 mL) and water (1.5 mL) were added a 12.5M aqueous sodium hydroxide solution (0.80 mL) and a solution of sodium hydroxide (0.26 g) in methanol (3.0 mL) at −30° C. Then, a solution of oxo(phenyl)acetaldehyde (1.0 g) in methanol (5.0 mL) was added, and the mixture was stirred at −20° C. for 2 hr and at room temperature for 1 hr. The reaction mixture was neutralized with acetic acid, and the resulting solid was collected by filtration and washed with water to give the title compound (0.86 g).

후처리

  1. customat −30° C
  2. filtrationthe resulting solid was collected by filtration
  3. washwashed with water

출처 및 근거

ORD 기록
ord-fc80dc711ee24038b3fe02f4bade722e
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09150588B2

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