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methyl (2R)-1-(N-{[(phenylmethyl)oxy]carbonyl}glycyl)-2-piperidinecarboxylate → (9aR)-octahydro-1H-pyrido(1,2-a)pyrazine-1,4-dione

HRID 1366594
ノート
印刷プレビュー

反応式

HRID 1366594 の反応式
C1(COC([NH:11][CH2:12][C:13]([N:15]2[CH2:20][CH2:19][CH2:18][CH2:17][C@@H:16]2[C:21]([O:23]C)=O)=[O:14])=O)C=CC=CC=1>CO>[C:21]1(=[O:23])[NH:11][CH2:12][C:13](=[O:14])[N:15]2[CH2:20][CH2:19][CH2:18][CH2:17][C@H:16]12
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 66936225methyl (2R)-1-(N-{[(phenylmethyl)oxy]carbonyl}glycyl)-2-piperidinecarboxylate

生成物 1

HCID 66936119(9aR)-octahydro-1H-pyrido(1,2-a)pyrazine-1,4-dione収率 76.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Methyl (2R)-1-(N-{[(phenylmethyl)oxy]carbonyl}glycyl)-2-piperidinecarboxylate (2.029 g, 6.068 mmol) was dissolved in MeOH (30 mL), degassed and placed under argon. 10% Pd/C (610 mg) was added, and the contents were thoroughly degassed and placed under a hydrogen balloon for 3 h. The contents were then degassed, and the Pd/C was removed by filtration through Celite, washing with MeOH. The filtrate was concentrated in vacuo to provide pure (9aR)-tetrahydro-2H-pyrido[1,2-a]pyrazine-1,4(3H,6H)-dione (779 mg, 76%). LCMS: (M+H)+: 169.1.

後処理

このページの内容参加物実験手順後処理出典と根拠反応ノート
  1. customdegassed
  2. addition10% Pd/C (610 mg) was added
  3. customthe contents were thoroughly degassed
  4. customfor 3 h
  5. customThe contents were then degassed
  6. customthe Pd/C was removed by filtration through Celite
  7. washwashing with MeOH
  8. concentrationThe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-448e1b1ef00645faab21406deed2153f
出典データセット
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07893056B2

反応ノート

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