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

HRID 1440018
ノート
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反応式

HRID 1440018 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 87885Chloromethyl pivalateHCID 23709643HCID 23709643、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-a3e97fd106d34e12aafd703dada50318
出典データセット
uspto-grants-1996_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05496949

反応ノート

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