Methyl 7-benzyl-5,6,7,8-tetrahydroimidazo[1,5-a]pyrazine-1-carboxylate → Methyl 5,6,7,8-tetrahydroimidazo[1,5-a]pyrazine-1-carboxylate

HRID 1808350ノート

反応式

HRID 1808350 の反応式
C([N:8]1[CH2:13][CH2:12][N:11]2[CH:14]=[N:15][C:16]([C:17]([O:19][CH3:20])=[O:18])=[C:10]2[CH2:9]1)C1C=CC=CC=1>CO>[C:16]1([C:17]([O:19][CH3:20])=[O:18])[N:15]=[CH:14][N:11]2[CH2:12][CH2:13][NH:8][CH2:9][C:10]=12

参加物

3

反応物 1

HCID 57635262Methyl 7-benzyl-5,6,7,8-tetrahydroimidazo[1,5-a]pyrazine-1-carboxylate

生成物 1

HCID 68508140Methyl 5,6,7,8-tetrahydroimidazo[1,5-a]pyrazine-1-carboxylate収率 99%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Methyl 7-benzyl-5,6,7,8-tetrahydroimidazo[1,5-a]pyrazine-1-carboxylate (3.69 mmol) was dissolved in MeOH (20 ml), and the solution was flushed with nitrogen. Pd(OH)2 (250 mg) and a cat. amount of AcOH were added, and the mixture was again flushed with nitrogen for 20 min. The reaction mixture was reacted under a hydrogen atmosphere (50 psi) for 5 h on a Parr hydrogenation apparatus. Filtration over Celite was then carried out, followed by washing with methanol. The resulting crude product was purified by column chromatography (silica gel, 3-5% MeOH in DCM), and the desired product was thus obtained in the form of a yellow solid. Yield: 99%

後処理

  1. customthe solution was flushed with nitrogen
  2. additionamount of AcOH were added
  3. customthe mixture was again flushed with nitrogen for 20 min
  4. customThe reaction mixture was reacted under a hydrogen atmosphere (50 psi) for 5 h on a Parr hydrogenation apparatus
  5. filtrationFiltration over Celite
  6. washby washing with methanol
  7. customThe resulting crude product was purified by column chromatography (silica gel, 3-5% MeOH in DCM)

出典と根拠

ORDレコード
ord-b3b1eafd5790499fa6d5dd526c1f1df9
出典データセット
uspto-grants-2013_01
特許番号
US08357717B2

反応ノート

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