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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
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HRID 1752503 반응식
[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]
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참가 물질

4

반응물 1

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

생성물 1

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

시약·촉매·용매 2

HCID 23938Palladium촉매2회HCID 702Ethanol용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-0381abb2503a4e06b54eaf8a21e1eb86
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09163011B2

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