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1,2-Dichloroethane → HCID 14625129、化合物

HRID 1904323
ノート
印刷プレビュー

反応式

HRID 1904323 の反応式
[N:1]1([CH2:7][C:8]2[CH:9]=[C:10]([CH:16]=[CH:17][CH:18]=2)[O:11][CH2:12][CH2:13][CH2:14][NH2:15])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[C:19]([S:22][CH2:23][C:24](O)=[O:25])(=[O:21])[CH3:20].C(Cl)CCl.O>ClCCl>[N:1]1([CH2:7][C:8]2[CH:9]=[C:10]([CH:16]=[CH:17][CH:18]=2)[O:11][CH2:12][CH2:13][CH2:14][NH:15][C:24](=[O:25])[CH2:23][S:22][C:19](=[O:21])[CH3:20])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 111,2-DichloroethaneHCID 962WaterHCID 14485Acetic acid, 2-(acetylthio)-HCID 102205613-(3-(Piperidin-1-ylmethyl)phenoxy)propan-1-amine

生成物 1

HCID 14625129HCID 14625129、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

2.94 g of 3-{3-(piperidinomethyl)phenoxy}propylamine was dissolved in 80 ml of dichloromethane, and stirred under cooling in an ice bath. 1.60 g of 2-(acetylthio)acetic acid and 2.26 g of EDC were added to this solution, and stirred at 0° C. for 30 minutes then at room temperature overnight. 100 ml of water and 50 ml of dichloromethane were added to the reaction solution, and extraction was carried out. The dichloromethane layer was washed twice with water, and dried over anhydrous magnesium sulfate. The solvent was evaporated in vacuo, and the residue was purified by silica gel column chromatography using methanol:dichloromethane=1:15 as developing solvent to obtain the colorless oily N-[3-{3-(piperidinomethyl)phenoxy}propyl]-2-(acetylthio)acetamide. Yield: 2.23 g.

後処理

  1. temperatureunder cooling in an ice bath
  2. stirringstirred at 0° C. for 30 minutes
  3. customat room temperature
  4. customovernight
  5. washThe dichloromethane layer was washed twice with water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customThe solvent was evaporated in vacuo
  8. customthe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-9a69c6c3a46444bc8a50cce25ff383bd
出典データセット
uspto-grants-1989_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04837316

反応ノート

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