Ethyl formate → HCID 20073630、化合物

HRID 704906ノート

反応式

HRID 704906 の反応式
Cl.[NH2:2][CH:3]([C:5]1([CH3:10])[O:9][CH2:8][CH2:7][O:6]1)[CH3:4].C[O-].[Na+].[CH:14](OCC)=[O:15]>CO>[CH:14]([NH:2][CH:3]([C:5]1([CH3:10])[O:9][CH2:8][CH2:7][O:6]1)[CH3:4])=[O:15]

参加物

5

反応物 3

HCID 8025Ethyl formateHCID 10942334Sodium MethoxideHCID 20073632HCID 20073632、化合物

生成物 1

HCID 20073630HCID 20073630、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

2-(1-Aminoethyl)-2-methyl-1,3-dioxolane hydrochloride (1.3 g, 0.0078 mol) was dissolved in methanol (25 ml). Sodium methoxide (25% w/w in methanol. 1.68 g, 0.0078 mol) was added and the suspension filtered through Celite. The Celite was rinsed with methanol (25 ml) and the combined filtrates had the solvent removed by rotary evaporation (25 Torr, 40° C.). The resulting clear oil was dissolved in ethyl formate (10.36 g. 0.14 mol) and heated to reflux under nitrogen. The reflux was continued for 4 hours. The excess ethyl formate and ethanol byproduct were removed by rotary evaporation (25 Torr, 40° C.) and the resulting solid was dried in vacuo (0.5 Torr, 25° C., 16 hours). The product was

後処理

  1. filtrationthe suspension filtered through Celite
  2. washThe Celite was rinsed with methanol (25 ml)
  3. customremoved by rotary evaporation (25 Torr, 40° C.)
  4. temperatureheated
  5. temperatureto reflux under nitrogen
  6. customThe excess ethyl formate and ethanol byproduct were removed by rotary evaporation (25 Torr, 40° C.)
  7. customthe resulting solid was dried in vacuo (0.5 Torr, 25° C., 16 hours)

出典と根拠

ORDレコード
ord-9160c386e03047528854ae3237ffd3ad
出典データセット
uspto-grants-1991_01
特許番号
US04988827

反応ノート

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