Potassium Carbonate → Ethyl 2-[4-(cyanomethoxy)phenyl]-2-ethoxycarbonylacetate

HRID 1901322노트

반응식

HRID 1901322 반응식
[CH2:1]([O:3][C:4]([CH:6]([C:12]1[CH:17]=[CH:16][C:15]([OH:18])=[CH:14][CH:13]=1)[C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:5])[CH3:2].Br[CH2:20][C:21]#[N:22].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[C:21]([CH2:20][O:18][C:15]1[CH:14]=[CH:13][C:12]([CH:6]([C:7]([O:9][CH2:10][CH3:11])=[O:8])[C:4]([O:3][CH2:1][CH3:2])=[O:5])=[CH:17][CH:16]=1)#[N:22]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 11534BromoacetonitrileHCID 12965552HCID 12965552, 화합물

생성물 1

HCID 21844455Ethyl 2-[4-(cyanomethoxy)phenyl]-2-ethoxycarbonylacetate수율 84.3%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

To 150 ml of acetone were added 14.58 g of ethyl 2-ethoxycarbonyl-2-(4-hydroxyphenyl)acetate, 8.8 g of bromoacetonitrile and 9.6 g of anhydrous potassium carbonate. After refluxing under heating for 5 hours, insoluble materials were removed by filtration, and the resulting filtrate was concentrated to dryness. The residue thus obtained was purified by silica gel column chromatography using toluene as an elution solvent, thereby obtaining 14.2 g of ethyl 2-[4-(cyanomethoxy)phenyl]-2-ethoxycarbonylacetate in the form of colorless oil.

후처리

  1. temperatureAfter refluxing
  2. temperatureunder heating for 5 hours
  3. custominsoluble materials were removed by filtration
  4. concentrationthe resulting filtrate was concentrated to dryness
  5. customThe residue thus obtained
  6. customwas purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-3c57b61027da4f3a884118d5c31aeb17
출처 데이터셋
uspto-grants-1996_11
특허 번호
US05576343

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