Triethyloxonium tetrafluoroborate → 1-[(2-Chlorophenyl)carbonyl]-3-(ethyloxy)piperazine

HRID 1888994ノート

反応式

HRID 1888994 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]([N:10]1[CH2:15][CH2:14][NH:13][C:12](=[O:16])[CH2:11]1)=[O:9].F[B-](F)(F)F.[CH2:22]([O+](CC)CC)[CH3:23]>ClCCl>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]([N:10]1[CH2:15][CH2:14][NH:13][CH:12]([O:16][CH2:22][CH3:23])[CH2:11]1)=[O:9]

参加物

4

反応物 2

HCID 2723982Triethyloxonium tetrafluoroborateHCID 310958254-[(2-Chlorophenyl)carbonyl]-2-piperazinone

生成物 1

HCID 675333581-[(2-Chlorophenyl)carbonyl]-3-(ethyloxy)piperazine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
25 °C

実験手順

4-[(2-chlorophenyl)carbonyl]-2-piperazinone (I4) (676 mg, 2.83 mmol) was dissolved in dichloromethane (DCM) (10 mL) and was treated with triethyloxonium tetrafluoroborate (628 mg, 3.31 mmol). The solution was stirred at 25° C. for 16 hr and the solution partitioned between ethyl acetate (25 mL) and saturated sodium bicarbonate solution (25 mL). The aqueous phase was extracted with ethyl acetate (3×25 mL), combined extracts were washed with brine (25 mL), dried over anhydrous sodium sulfate and concentrated to a crude oil in 816 mg that was used in the subsequent step without further purification. Compound was not characterised but used directly in the next step.

後処理

  1. customthe solution partitioned between ethyl acetate (25 mL) and saturated sodium bicarbonate solution (25 mL)
  2. extractionThe aqueous phase was extracted with ethyl acetate (3×25 mL)
  3. washwere washed with brine (25 mL)
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated to a crude oil in 816 mg that
  6. customwas used in the subsequent step without further purification

出典と根拠

ORDレコード
ord-14bb6c053b484a4e90b40085625e7b2a
出典データセット
uspto-grants-2013_08
特許番号
US08501946B2

反応ノート

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