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 1808350노트

반응식

HRID 1808350 반응식
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

참가 물질

3

반응물 1

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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%

후처리

  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)

출처 및 근거

ORD 기록
ord-b3b1eafd5790499fa6d5dd526c1f1df9
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08357717B2

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