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Water → N-[2-(2-benzo[b]thiophen-5-ylethoxy)ethyl]-N,N-dipropylamine

HRID 1007893
ノート
印刷プレビュー

反応式

HRID 1007893 の反応式
CS(O[CH2:6][CH2:7][O:8][CH2:9][CH2:10][C:11]1[CH:19]=[CH:18][C:14]2[S:15][CH:16]=[CH:17][C:13]=2[CH:12]=1)(=O)=O.[CH2:20]([NH:23][CH2:24][CH2:25][CH3:26])[CH2:21][CH3:22].C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O.C(OCC)(=O)C>[S:15]1[CH:16]=[CH:17][C:13]2[CH:12]=[C:11]([CH2:10][CH2:9][O:8][CH2:7][CH2:6][N:23]([CH2:24][CH2:25][CH3:26])[CH2:20][CH2:21][CH3:22])[CH:19]=[CH:18][C:14]1=2
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 962WaterHCID 8902DipropylamineHCID 11430Potassium CarbonateHCID 219900502-(2-Benzo[b]thiophen-5-ylethoxy)ethyl methanesulfonate

生成物 1

HCID 22666418N-[2-(2-benzo[b]thiophen-5-ylethoxy)ethyl]-N,N-dipropylamine

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
80 °C

実験手順

In 8 mL of N,N-dimethylformamide is dissolved 0.80 g of 2-(2-benzo[b]thiophen-5-ylethoxy)ethyl methanesulfonate, to which are added 0.73 mL of dipropylamine and 0.74 g of potassium carbonate. The resulting mixture is stirred at 80° C. for 3 hours. The reaction mixture is introduced into a mixture of water and ethyl acetate, and the organic layer is separated. The organic layer is washed with water and saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate, the solvent is distilled off under reduced pressure, and the residue is purified by column chromatography (eluent:chloroform:methanol=10:1). Thus, 0.60 of N-[2-(2-benzo[b]thiophen-5-ylethoxy)ethyl]-N,N-dipropylamine is obtained as an oily product.

後処理

  1. customthe organic layer is separated
  2. washThe organic layer is washed with water and saturated aqueous solution of sodium chloride
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationthe solvent is distilled off under reduced pressure
  5. customthe residue is purified by column chromatography (eluent:chloroform:methanol=10:1)

出典と根拠

ORDレコード
ord-57cac10567b94557a233ed95646d8627
出典データセット
uspto-grants-2004_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06797726B1

反応ノート

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