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Trifluoroacetic acid → 2-aminoethyl acetate TFA-salt

HRID 1349005
ノート
印刷プレビュー

反応式

HRID 1349005 の反応式
C([CH:8]([CH2:10][NH2:11])O)(OC(C)(C)C)=O.[C:12]([OH:18])([C:14]([F:17])([F:16])[F:15])=[O:13]>C(Cl)Cl>[OH:18][C:12]([C:14]([F:17])([F:16])[F:15])=[O:13].[C:12]([O:18][CH2:8][CH2:10][NH2:11])(=[O:13])[CH3:14]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 22707757Propanoic acid, 3-amino-2-hydroxy-, 1,1-dimethylethyl ester

生成物 1

HCID 873085332-aminoethyl acetate TFA-salt

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution was made containing ethanolamine (36.5 ml, 0.6 mol) in chloroform (1000 ml). The Boc2O (13.1 g, 60 mmol) dissolved in chloroform (600 ml) was slowly added dropwise at 0° C. over a 6-hours period (the temperature was maintained all over this period). The reaction was allowed to reach room temperature and was stirred overnight. The organic layer was washed with water (2×500 ml), brine and dried over magnesium sulfate before being concentrated in vacuo. The desired product (9.5 g,>95%) was isolated as a colourless oil and was used without further purification. A solution was made containing the Boc-ethanolamine (1.92 g, 12 mmol) with potassium carbonate (5 g, 36 mmol) in DCM (40 ml). Acetyl chloride (30 ml, 0.42 mol) was added and the reaction stirred for 6 hours at room temperature. The excess of acetyl chloride was removed in vacuo and the crude dissolved in DCM (100 ml). The organic layer was washed with water (50 ml), brine and dried over magnesium sulfate before being concentrated in vacuo. The desired product (1.86 g, 77%) was isolated as a colourless oil and was used without further purification. A solution was made containing the O-acyl, Boc-ethanolamine (1.65 g, 8.1 mmol) in DCM (20 ml) and TFA (20 ml) was added. After one hour at room temperature, the solvent was removed in vacuo. The crude was concentrated from methanol (2–3 times) and from DCM (2–3 times) to give the expected compound (1.75 g, quant.) as an oil used without further purification.

後処理

  1. customwas used without further purification
  2. additionwas added
  3. customthe solvent was removed in vacuo
  4. concentrationThe crude was concentrated from methanol (2–3 times) and from DCM (2–3 times)

出典と根拠

ORDレコード
ord-0a83f236aca54e71ab2448e5afa22057
出典データセット
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07211601B2

反応ノート

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