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Water → 4,5-Diethyloxazol-2-amine

HRID 421029
ノート
印刷プレビュー

反応式

HRID 421029 の反応式
[CH3:1][CH2:2][C:3](=O)[CH:4]([CH2:6][CH3:7])[OH:5].[N:9]#[C:10][NH2:11].[O-]CC.[Na+].O>C(O)C>[NH2:11][C:10]1[O:5][C:4]([CH2:6][CH3:7])=[C:3]([CH2:2][CH3:1])[N:9]=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 962WaterHCID 9864CyanamideHCID 956094-Hydroxyhexan-3-oneHCID 2723922Sodium ethoxide

生成物 1

HCID 178601934,5-Diethyloxazol-2-amine収率 31.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Propioin (1.03 g, 8.37 mmol) was dissolved in ethanol (15 mL). Cyanamide (0.75 g, 17.7 mmol) and sodium ethoxide (1.21 g, 17.7 mmol) were added, and the mixture was stirred at room temperature for 3.5 hours. The reaction mixture was poured into water and extracted with ethyl acetate. After the organic layer was washed with water and brine, dried over anhydrous sodium sulfate, the residue obtained by evaporation under reduced pressure was purified by chromatography on silica gel (dichloromethane:methanol=9:1) to give the title compound (369.2 mg, 29.7%) as a yellow amorphous.

後処理

  1. extractionextracted with ethyl acetate
  2. washAfter the organic layer was washed with water and brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customthe residue obtained by evaporation under reduced pressure
  5. customwas purified by chromatography on silica gel (dichloromethane:methanol=9:1)

出典と根拠

ORDレコード
ord-dc9178b141b9494d9295114ee8c3f8ba
出典データセット
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08097759B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート