Ethanolamine → HCID 69004593, 화합물

HRID 1436089노트

반응식

HRID 1436089 반응식
[CH3:1][C:2]([C:4]1[CH:9]=[C:8]([F:10])[C:7]([F:11])=[C:6]([F:12])[CH:5]=1)=O.[CH2:13]([CH2:15][NH2:16])[OH:14]>C1(C)C=CC=CC=1>[F:12][C:6]1[CH:5]=[C:4]([CH:2]([NH:16][CH2:15][CH2:13][OH:14])[CH3:1])[CH:9]=[C:8]([F:10])[C:7]=1[F:11]

참가 물질

4

반응물 2

HCID 700EthanolamineHCID 27769073',4',5'-Trifluoroacetophenone

생성물 1

HCID 69004593HCID 69004593, 화합물수율 34.2%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture of 3,4,5-trifluoroacetophenone (2.0 g), ethanolamine (2.0 g), and toluene (20 mL) was heated under reflux in a Dean-Stark apparatus for 2.5 hours. The reaction solution was concentrated under reduced pressure, and then the residue was diluted with ethanol (30 mL) and sodium borohydride (1.0 g) was added under ice-cooling. The mixture was stirred at room temperature for three hours and then diluted with a 2 N sodium hydroxide solution and chloroform. Thereafter, the organic layer was separated. The organic layer was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The residue was purified by column chromatography using a silica gel (chloroform:methanol=50:1 to 5:1) to obtain 860 mg of the title compound.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux in a Dean-Stark apparatus for 2.5 hours
  3. concentrationThe reaction solution was concentrated under reduced pressure
  4. additionthe residue was diluted with ethanol (30 mL) and sodium borohydride (1.0 g)
  5. additionwas added under ice-
  6. temperaturecooling
  7. additiondiluted with a 2 N sodium hydroxide solution and chloroform
  8. customThereafter, the organic layer was separated
  9. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  10. concentrationconcentrated under reduced pressure
  11. customThe residue was purified by column chromatography

출처 및 근거

ORD 기록
ord-89e3608ba1bf452e80ae1995ea951a1b
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07618960B2

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