Water → HCID 178518202, 화합물

HRID 271396

반응식

HRID 271396 반응식
[Na].[C:2]1([CH:8]([C:12]([NH2:14])=[O:13])[C:9]([NH2:11])=[O:10])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH:15](OCC)=O.O>C(O)C>[C:2]1([C:8]2[C:12]([OH:13])=[N:14][CH:15]=[N:11][C:9]=2[OH:10])[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 8025Ethyl formateHCID 27475362-PhenylmalonamideHCID 5360545Sodium

생성물 1

HCID 178518202HCID 178518202, 화합물수율 69.1%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
50 °C

실험 절차

Sodium metal (0.92 g, 40 mmol) was dissolved by stirring in ethanol (30 mL) at room temperature under argon over 40 min. To the resulting solution at room temperature was added 2-phenylmalonamide (3.56 g, 20 mmol) and ethyl formate (1.9 mL, 24 mmol). The resulting suspension was heated at 50° C. under argon 16 h. After cooling the reaction mixture to room temperature, water (100 mL) was added and the mixture was stirred for 1 h. Solid was removed by filtration. The filtrate was acidified to pH˜4 with 1 M aqueous HCl. The resulting precipitate was collected by filtration and further washed with water (20 mL×2), then Et2O (10 mL×2). After drying under vacuum for 3 h, the title compound (2.6 g) was obtained as a light yellow solid. HPLC/MS: retention time=0.76 min, [M+H]+=189.

후처리

  1. temperatureAfter cooling the reaction mixture to room temperature
  2. customSolid was removed by filtration
  3. filtrationThe resulting precipitate was collected by filtration
  4. washfurther washed with water (20 mL×2)
  5. customAfter drying under vacuum for 3 h

출처 및 근거

ORD 기록
ord-688288197ef7443e83e0b009843faba2
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07452892B2

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