Ethyl Acetate → HCID 57927460, 화합물

HRID 889154노트

반응식

HRID 889154 반응식
[O:1]1[CH:5]=[C:4]([C:6]([NH:8][NH2:9])=[O:7])[N:3]=[CH:2]1.CCCCCCC.[C:17](OCC)(=[O:19])C>ClC(OC(Cl)(Cl)Cl)=O>[O:1]1[CH:5]=[C:4]([C:6]2[O:7][C:17](=[O:19])[NH:9][N:8]=2)[N:3]=[CH:2]1

참가 물질

5

반응물 3

HCID 8857Ethyl AcetateHCID 8900HeptaneHCID 497617151,3-Oxazole-4-carbohydrazide

생성물 1

HCID 57927460HCID 57927460, 화합물

시약·촉매·용매 1

HCID 10426Diphosgene용매

실험 절차

After suspending oxazole-4-carboxylic acid hydrazide (CAS 885274-12-4) (1.06 g) in ethyl acetate (10 ml), trichloromethyl chloroformate (1.21 ml) was added dropwise while stirring on ice. Upon completion of the dropwise addition, the mixture was heated to reflux for 2 hours and 20 minutes. It was then allowed to cool, n-heptane was added to the reaction mixture, and the precipitate was collected by filtration. The filtrate was concentrated under reduced pressure and the residue was recrystallized with toluene-ethyl acetate. This was combined with the previously filtered substance to obtain the title compound (1.38 g).

후처리

  1. additionwas added dropwise
  2. additionUpon completion of the dropwise addition
  3. temperaturethe mixture was heated
  4. temperatureto reflux for 2 hours and 20 minutes
  5. temperatureto cool
  6. filtrationthe precipitate was collected by filtration
  7. concentrationThe filtrate was concentrated under reduced pressure
  8. customthe residue was recrystallized with toluene-ethyl acetate

출처 및 근거

ORD 기록
ord-f410baf8e0504ce09ec5f5587acf8550
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08252810B2

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