Ethyl chloroformate → Carbamic acid, N-(cyanomethyl)-, ethyl ester

HRID 1418707노트

반응식

HRID 1418707 반응식
S(O)(O)(=O)=O.[NH2:6][CH2:7][C:8]#[N:9].[OH-].[Na+].Cl[C:13]([O:15][CH2:16][CH3:17])=[O:14]>O>[C:8]([CH2:7][NH:6][C:13](=[O:14])[O:15][CH2:16][CH3:17])#[N:9]

참가 물질

5

반응물 3

HCID 10928Ethyl chloroformateHCID 14798Sodium Hydroxide4회HCID 196971Aminoacetonitrile sulfate (1:1)

생성물 1

HCID 83704Carbamic acid, N-(cyanomethyl)-, ethyl ester수율 97%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Aminoacetonitrile sulfate (H2NCH2CN.1/2H2SO4, 121.5 g, 1.156mole) was dissolved in water (230.9 g) and the solution was cooled to 0° to 5° C. and adjusted to pH 5 to 7 by the addition of a small amount of 30% aqueous sodium hydroxide solution. Ethyl chloroformate (108.5 g, 1.00 mole) and 30% aqueous sodium hydroxide solution were concurrently added dropwise with stirring and keeping pH at 5 to 7 at 0° to 5° C. over 2 hours and the mixture was stirred at the same temperature for additional 2 hours while keeping the same pH by dropping, if necessary, 30% aqueous sodium hydroxide solution. The total amount of 30% aqueous sodium hydroxide solution was 294.3 g. The reaction mixture was extracted three times with toluene (485 ml). The toluene layer was dried over anhydrous magnesium sulfate, toluene was evaporated and the residue was cooled to room temperature to give crystals (124.7 g, 0.968 mole) of ethyl N-cyanomethylcarbamate.

후처리

  1. temperaturethe solution was cooled to 0° to 5° C.
  2. customat 0° to 5° C.
  3. customover 2 hours
  4. stirringthe mixture was stirred at the same temperature for additional 2 hours
  5. extractionThe reaction mixture was extracted three times with toluene (485 ml)
  6. dry with materialThe toluene layer was dried over anhydrous magnesium sulfate, toluene
  7. customwas evaporated

출처 및 근거

ORD 기록
ord-497022630c1f4e958d92caf3f54fefa2
출처 데이터셋
uspto-grants-1999_03
특허 번호
US05883260

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