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

HRID 548708ノート

反応式

HRID 548708 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-12045789a31b42b6861539732f48df04
出典データセット
uspto-grants-2011_05
特許番号
US07943607B2

反応ノート

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