Acetamidine monohydrochloride → HCID 136043557, 화합물

HRID 1742023

반응식

HRID 1742023 반응식
Cl.[C:2]([NH2:5])(=[NH:4])[CH3:3].[F:6][C:7]([F:20])([C:16]([F:19])([F:18])[F:17])[C:8]([CH2:10][C:11](OCC)=[O:12])=O>CCO>[CH3:3][C:2]1[NH:5][C:11](=[O:12])[CH:10]=[C:8]([C:7]([F:6])([F:20])[C:16]([F:17])([F:18])[F:19])[N:4]=1

참가 물질

4

반응물 2

HCID 67170Acetamidine monohydrochlorideHCID 522203Ethyl 4,4,5,5,5-Pentafluoro-3-oxovalerate

생성물 1

HCID 136043557HCID 136043557, 화합물수율 52.6%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of Na (2.3 g, 0.1 mol) in EtOH (125 mL) was mixed with acetamidine hydrochloride (4.72 g, 50 mmol) and the reaction mixture was stirred for 15 min. Ethyl pentafluoropropionylacetate (11.7 g, 50 mmol) was added and the reaction mixture was refluxed for 6 h. The solvent was removed in vacuo, and the residue was taken up in H2O and acidified with dilute HCl to pH 2. The aqueous solution was extracted with EtOAc and the organic layer was dried over Na2SO4, then evaporated to afford 6 g of a yellowish solid. The crude product was purified by flash chromatography (CHCl3 containing MeOH 0% to 4%) to provide 2 g (17.5% yield) of a solid.

후처리

  1. temperaturethe reaction mixture was refluxed for 6 h
  2. customThe solvent was removed in vacuo
  3. extractionThe aqueous solution was extracted with EtOAc
  4. dry with materialthe organic layer was dried over Na2SO4
  5. customevaporated

출처 및 근거

ORD 기록
ord-74bdcbd4ca6548bdb9315a916f76d485
출처 데이터셋
uspto-grants-1994_08
특허 번호
US05336677

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