Diethyl Ether → HCID 15065506、化合物

HRID 846659ノート

反応式

HRID 846659 の反応式
[CH3:1][N:2]=[C:3]=[O:4].C(O[CH:8](OCC)[CH2:9][NH:10][CH2:11][C:12]#[CH:13])C.[CH3:17]COCC>>[CH3:1][N:2]1[CH:8]=[CH:9][N:10]([CH:11]([CH3:17])[C:12]#[CH:13])[C:3]1=[O:4]

参加物

4

反応物 3

HCID 3283Diethyl EtherHCID 12228Methyl IsocyanateHCID 15065591HCID 15065591、化合物

生成物 1

HCID 15065506HCID 15065506、化合物

反応条件

温度
50 °C

実験手順

Methyl isocyanate (4.6 g, 0.081 mol) was added to a stirred solution of 2,2-diethoxy-N-(2-propynyl)ethylamine (13.7 g, 0.074 mol) in ether (150 mL). After 30 min the ether was evaporated and the residue was dissolved in water (150 mL), oxalic acid (6.7 g) was added, and the solution was heated at 50° C. for 30 min. The solution was then concentrated to 20 mL and neutralized with 4N NaOH solution, and extracted with ethyl acetate (4×150 mL). The ethyl acetate was evaporated and the residue was chromatographed on silica gel to give 9.6 g of product as an oil.

後処理

  1. customAfter 30 min the ether was evaporated
  2. dissolutionthe residue was dissolved in water (150 mL)
  3. additionoxalic acid (6.7 g) was added
  4. concentrationThe solution was then concentrated to 20 mL and neutralized with 4N NaOH solution
  5. extractionextracted with ethyl acetate (4×150 mL)
  6. customThe ethyl acetate was evaporated
  7. customthe residue was chromatographed on silica gel

出典と根拠

ORDレコード
ord-479bca9d1d59462aa80ee37a1c9c18ff
出典データセット
uspto-grants-1992_08
特許番号
US05137905

反応ノート

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