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Dimethylformamide → Pyrazinecarboxylic acid, (2,2-dimethyl-1-oxopropoxy)methyl ester

HRID 1440018
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HRID 1440018 반응식
[N:1]1[CH:6]=[CH:5][N:4]=[CH:3][C:2]=1[C:7]([O-:9])=[O:8].[Na+].[C:11]([O:17][CH2:18]Cl)(=[O:16])[C:12]([CH3:15])([CH3:14])[CH3:13].CN(C)C=O>C1(C)C=CC=CC=1>[N:1]1[CH:6]=[CH:5][N:4]=[CH:3][C:2]=1[C:7]([O:9][CH2:18][O:17][C:11](=[O:16])[C:12]([CH3:15])([CH3:14])[CH3:13])=[O:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 87885Chloromethyl pivalateHCID 23709643HCID 23709643, 화합물

생성물 1

HCID 10331752Pyrazinecarboxylic acid, (2,2-dimethyl-1-oxopropoxy)methyl ester수율 78%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A four-necked flask was charged with 127.5 g (0.873 mole) of sodium pyrazinecarboxylate, 119.3 g (0.792 mole) of chloromethyl pivalate and 146 g of dimethylformamide and the internal temperature was maintained under stirring at 105°-110° C. for 8 hours. The reaction mixture was then cooled and transferred to a separatory funnel. After addition of 500 g of toluene, the mixture was washed with 3 portions, or a total of 900 g, of water. From the toluene layer which separated the toluene was first distilled off and the residue was subjected to distillation under reduced pressure to give 147 g of pivaloyloxymethyl pyrazinecarboxylate. Yield: 78% (based on chloromethyl pivalate).

후처리

  1. temperaturethe internal temperature was maintained
  2. temperatureThe reaction mixture was then cooled
  3. customtransferred to a separatory funnel
  4. washthe mixture was washed with 3 portions
  5. customFrom the toluene layer which separated the toluene
  6. distillationwas first distilled off
  7. distillationthe residue was subjected to distillation under reduced pressure

출처 및 근거

ORD 기록
ord-a3e97fd106d34e12aafd703dada50318
출처 데이터셋
uspto-grants-1996_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05496949

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