Ethyl formate → HCID 20073630, 화합물

HRID 704906노트

반응식

HRID 704906 반응식
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]

참가 물질

5

반응물 3

HCID 8025Ethyl formateHCID 10942334Sodium MethoxideHCID 20073632HCID 20073632, 화합물

생성물 1

HCID 20073630HCID 20073630, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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

후처리

  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)

출처 및 근거

ORD 기록
ord-9160c386e03047528854ae3237ffd3ad
출처 데이터셋
uspto-grants-1991_01
특허 번호
US04988827

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