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Water → 2-(2-Piperazin-1-ylethoxy)acetamide

HRID 1383751
ノート
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反応式

HRID 1383751 の反応式
Cl[CH2:2][CH2:3][O:4][CH2:5][C:6]([NH2:8])=[O:7].[NH:9]1[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]1.O>C1(C)C=CC=CC=1>[N:9]1([CH2:2][CH2:3][O:4][CH2:5][C:6]([NH2:8])=[O:7])[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 4837PiperazineHCID 110189312-(2-Chloroethoxy)acetamide

生成物 1

HCID 211883622-(2-Piperazin-1-ylethoxy)acetamide収率 39.5%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of 13.15 g of (2-chloroethoxy)acetamide (0.1 mol) and 43 g of anhydrous piperazine (0.5 mol) in 250 ml of toluene is introduced into a round-bottomed flask fitted with a water-cooled condenser and a mechanical stirrer. The mixture is heated at the reflux temperature for 4 hours. The precipitate formed is filtered off while hot and the solvent of the filtrate is evaporated off under reduced pressure to dryness. The evaporation residue is purified by chromatography on silica gel (eluent: 14/5/1 (v/v/v) of dichloromethane/methanol/28% aqueous ammonia solution). 7.4 g of 2-[2-(1-piperazinyl)ethoxy]acetamide are obtained in the form of a yellow oil. Yield: 39% Mass spectrum: 188 (MH+), 99 (HN(C4H8)N+=CH2), 44 (CONH2).

後処理

  1. additionis introduced into a round-bottomed flask
  2. temperaturecooled condenser and a mechanical stirrer
  3. temperatureThe mixture is heated at the reflux temperature for 4 hours
  4. customThe precipitate formed
  5. filtrationis filtered off while hot and the solvent of the filtrate
  6. customis evaporated off under reduced pressure to dryness
  7. customThe evaporation residue is purified by chromatography on silica gel (eluent: 14/5/1 (v/v/v) of dichloromethane/methanol/28% aqueous ammonia solution)

出典と根拠

ORDレコード
ord-02214f4e121e4dc189ef496d532ac9ab
出典データセット
uspto-grants-2001_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06255487B1

反応ノート

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