Water → HCID 70197198, 화합물

HRID 1419855노트

반응식

HRID 1419855 반응식
[Na].[C:2]([CH2:4][C:5]1[CH:10]=[C:9]([CH3:11])[CH:8]=[CH:7][N:6]=1)#[N:3].[Cl:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=1[CH:19](CO)[C:20]([OH:22])=O.[OH2:25]>CO>[Cl:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=1[CH:19]1[C:20](=[O:22])[C:4]([C:5]2[CH:10]=[C:9]([CH3:11])[CH:8]=[CH:7][N:6]=2)=[C:2]([NH2:3])[O:25]1

참가 물질

6

반응물 4

HCID 962WaterHCID 5360545Sodium2회HCID 12812206(4-Methylpyridin-2-yl)acetonitrileHCID 53970006HCID 53970006, 화합물

생성물 1

HCID 70197198HCID 70197198, 화합물수율 28%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Sodium (0.35 g, 15.2 mmol) was added in methanol (8 ml) and stirred at room temperature under nitrogen atomsphere till complete dissolution of sodium, and then 2-cyanomethyl-4-methylpyridine (1.10 g, 8.51 mmol) and 2-(o-chlorophenyl)2-hydroxymethylacetic acid (1.78 g, 1.35 mmol) were slowly added. After refluxing for 2 hours with stirring the solution was cooled with a small amount of water and concentrated under the reduced pressure. The residue was extracted with methylene chloride and the combined organic layers were dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure to get crude product. The residue was separated and purified by column-chromatography over silica gel to obtain the desired product (0.54 g, yield=28%).

후처리

  1. temperatureAfter refluxing for 2 hours
  2. concentrationconcentrated under the reduced pressure
  3. extractionThe residue was extracted with methylene chloride
  4. dry with materialthe combined organic layers were dried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customto get crude product
  8. customThe residue was separated
  9. custompurified by column-chromatography over silica gel

출처 및 근거

ORD 기록
ord-f7b3f025afa041d9be10309080f63d0f
출처 데이터셋
uspto-grants-1999_03
특허 번호
US05889027

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