Methyl chloroformate → Methyl N-(iminomethoxymethyl)carbamate

HRID 126906

반응식

HRID 126906 반응식
S(O)(O)(=O)=O.[CH3:6][O:7][C:8](=[NH:10])[NH2:9].[CH3:11][O:12][C:13](Cl)=[O:14].[OH-].[Na+]>O>[CH3:11][O:12][C:13]([NH:10][C:8](=[NH:9])[O:7][CH3:6])=[O:14]

참가 물질

5

반응물 3

HCID 6586Methyl chloroformateHCID 14798Sodium HydroxideHCID 169039Carbamimidic acid, methyl ester, sulfate (1:1)

생성물 1

HCID 137319931Methyl N-(iminomethoxymethyl)carbamate

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

246 g of O-methylisourea sulfate are dissolved in 300 ml of water and 163 ml of chloroformic acid methyl ester are added dropwise at 10° C., followed by 170 g of NaOH, dissolved in 510 ml of water. The mixture is stirred at room temperature for a further 3 hours. The reaction solution is then extracted with ethyl acetate and this extract is dried with anhydrous sodium sulfate. Evaporation under reduced pressure at a maximum bath temperature of 40° C. gives the N-methoxycarbonyl-O-methylisourea as an oil, which gradually solidifies to form crystals with a melting point of 40° C. Yield 150 g.

후처리

  1. extractionThe reaction solution is then extracted with ethyl acetate
  2. dry with materialthis extract is dried with anhydrous sodium sulfate
  3. customEvaporation under reduced pressure at a maximum bath temperature of 40° C.

출처 및 근거

ORD 기록
ord-6b9117b65bf24eb2a443470fd78e9f40
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04254143

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