Triethylamine → 1-(Methoxymethyl)-1H-imidazole-2-carboxylic acid

HRID 261949

반응식

HRID 261949 반응식
Cl[C:2]([O:4]CC)=[O:3].[CH3:7][O:8][CH2:9][N:10]1[CH:14]=[CH:13][N:12]=[CH:11]1.C(N(CC)CC)C>C(Cl)(Cl)Cl>[CH3:7][O:8][CH2:9][N:10]1[CH:14]=[CH:13][N:12]=[C:11]1[C:2]([OH:4])=[O:3]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 883591-(methoxymethyl)-1H-imidazole

생성물 1

HCID 219727271-(Methoxymethyl)-1H-imidazole-2-carboxylic acid

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
0 °C

실험 절차

At a temperature of -10° C., 27.5 g. (0.25 mol) of ethyl chloroformate was added drop-wise to a solution of 28 g. (0.25 mol) of 1-(methoxymethyl)imidazole and 25 g. (0.25 mol) of triethylamine in 125 ml. of anhydrous chloroform. The mixture was stirred at 0° C. and then kept standing for two days at room temperature. The precipitated triethylamine hydrochloride was filtered off and washed with diethyl ether. The filtrate was concentrated by evaporating the solvents and the residue was dissolved in diethyl ether. The solution was dried over sodium sulphate, the ether was distilled off and the residue was distilled. The ethyl ester of 1-(methoxymethyl)imidazole-2-carboxylic acid was obtained. Boiling point 120°-124°/2 mm. Hg.

후처리

  1. customAt a temperature of -10° C., 27.5 g
  2. filtrationThe precipitated triethylamine hydrochloride was filtered off
  3. washwashed with diethyl ether
  4. concentrationThe filtrate was concentrated
  5. customby evaporating the solvents
  6. dissolutionthe residue was dissolved in diethyl ether
  7. dry with materialThe solution was dried over sodium sulphate
  8. distillationthe ether was distilled off
  9. distillationthe residue was distilled

출처 및 근거

ORD 기록
ord-e60a0c7e7e694c77a827280a22a9cff3
출처 데이터셋
uspto-grants-1979_05
특허 번호
US04152441

연결된 노트

불러오는 중…