Acetamidine monohydrochloride → HCID 136043557、化合物

HRID 1742023

反応式

HRID 1742023 の反応式
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

参加物

4

反応物 2

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

生成物 1

HCID 136043557HCID 136043557、化合物収率 52.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-74bdcbd4ca6548bdb9315a916f76d485
出典データセット
uspto-grants-1994_08
特許番号
US05336677

関連ノート

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