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3-Amino-5-(2-methoxy-vinyl)-pyrazine-2-carboxylic acid methyl ester → 3-Amino-5-(2-methoxy-ethyl)-pyrazine-2-carboxylic acid methyl ester

HRID 1752503
ノート
印刷プレビュー

反応式

HRID 1752503 の反応式
[CH3:1][O:2][C:3]([C:5]1[C:10]([NH2:11])=[N:9][C:8]([CH:12]=[CH:13][O:14][CH3:15])=[CH:7][N:6]=1)=[O:4]>CCO.[Pd]>[CH3:1][O:2][C:3]([C:5]1[C:10]([NH2:11])=[N:9][C:8]([CH2:12][CH2:13][O:14][CH3:15])=[CH:7][N:6]=1)=[O:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 780595033-Amino-5-(2-methoxy-vinyl)-pyrazine-2-carboxylic acid methyl ester

生成物 1

HCID 712711513-Amino-5-(2-methoxy-ethyl)-pyrazine-2-carboxylic acid methyl ester収率 56.1%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒2 回HCID 702Ethanol溶媒

実験手順

A solution of 3-amino-5-(2-methoxy-vinyl)-pyrazine-2-carboxylic acid methyl ester (260 mg, 1.24 mmol) and Pd/C 10% (50 mg) in EtOH (10 ml) was stirred at rt and under an atmosphere of hydrogen for 17 h. To complete the reaction, more Pd/C 10% (84 mg) was added and the reaction was stirred under an atmosphere of hydrogen for 37 h. The suspension was filtered off and washed with EtOH and then residual solution was evaporated. The residue was purified by chromatography on silica gel (DCM to DCM/MeOH 9:1) to provide the title compound as yellow solid (147 mg).

後処理

  1. additionwas added
  2. filtrationThe suspension was filtered off
  3. washwashed with EtOH
  4. customresidual solution was evaporated
  5. customThe residue was purified by chromatography on silica gel (DCM to DCM/MeOH 9:1)

出典と根拠

ORDレコード
ord-0381abb2503a4e06b54eaf8a21e1eb86
出典データセット
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09163011B2

反応ノート

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