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

HRID 1440016
ノート
印刷プレビュー

反応式

HRID 1440016 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].C(N(CC)CC)C>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 8471TriethylamineHCID 87885Chloromethyl pivalateHCID 23709643HCID 23709643、化合物

生成物 1

HCID 10331752Pyrazinecarboxylic acid, (2,2-dimethyl-1-oxopropoxy)methyl ester収率 72.2%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A four-necked flask was charged with 14.6 g (0.10 mole) of sodium pyrazinecarboxylate, 15.1 g (0.10 mole) of chloromethyl pivalate and 1.0 g (0.01 mole) of triethylamine and the charge was maintained under stirring at 98°-100° C. for 6 hours. The reaction mixture was then cooled and 100 ml of toluene was added. The solids (sodium chloride) were filtered off. From the filtrate thus obtained the toluene was distilled off and the filtrate was subjected to distillation under reduced pressure to give 17.2 g of pivaloyloxymethyl pyrazinecarboxylate. Yield: 72%

後処理

  1. temperaturethe charge was maintained
  2. temperatureThe reaction mixture was then cooled
  3. filtrationThe solids (sodium chloride) were filtered off
  4. customFrom the filtrate thus obtained the toluene
  5. distillationwas distilled off
  6. distillationthe filtrate was subjected to distillation under reduced pressure

出典と根拠

ORDレコード
ord-4ad07fb905c94c119f988e96b78b1c4c
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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