2-(Methylamino)ethanol → 2,4,5-trifluoro-N-(2-hydroxyethyl)-N-methylbenzamide

HRID 548708노트

반응식

HRID 548708 반응식
[F:1][C:2]1[CH:10]=[C:9]([F:11])[C:8]([F:12])=[CH:7][C:3]=1[C:4](Cl)=[O:5].[CH3:13][NH:14][CH2:15][CH2:16][OH:17]>C(Cl)Cl.[OH-].[Na+]>[F:1][C:2]1[CH:10]=[C:9]([F:11])[C:8]([F:12])=[CH:7][C:3]=1[C:4]([N:14]([CH2:15][CH2:16][OH:17])[CH3:13])=[O:5]

참가 물질

5

반응물 2

HCID 80162-(Methylamino)ethanolHCID 1451642,4,5-Trifluorobenzoyl chloride

생성물 1

HCID 576631992,4,5-trifluoro-N-(2-hydroxyethyl)-N-methylbenzamide수율 105.8%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 14798Sodium Hydroxide용매

실험 절차

2,4,5-Trifluorobenzoyl chloride (540 mg, 2.78 mmol) was added to a stirred solution of 2-methylaminoethanol (0.185 mL, 3.06 mmol) in DCM (5 mL) and 10% aqueous sodium hydroxide solution (5 mL) at 0° C. After addition was complete the icebath was removed and the reaction was allowed to warm up to RT and stirred for 3 hours. The phases were then separated and the aqueous phase extracted with DCM (3×30 mL). The combined organic layers were dried (MgSO4), filtered and evaporated to give the desired compound as a colourless oil (686 mg). This material was used without further purification.

후처리

  1. additionAfter addition
  2. customwas removed
  3. customThe phases were then separated
  4. extractionthe aqueous phase extracted with DCM (3×30 mL)
  5. dry with materialThe combined organic layers were dried (MgSO4)
  6. filtrationfiltered
  7. customevaporated

출처 및 근거

ORD 기록
ord-12045789a31b42b6861539732f48df04
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07943607B2

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