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Tert-butyl 3-(2-(((benzyloxy)carbonyl)(methyl)amino)acetamido)azetidine-1-carboxylate → Tert-butyl 3-(2-(methylamino)acetamido)azetidine-1-carboxylate

HRID 1896892
ノート
印刷プレビュー

反応式

HRID 1896892 の反応式
C(O[C:9]([N:11](C)[CH2:12][C:13]([NH:15][CH:16]1[CH2:19][N:18]([C:20]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[O:21])[CH2:17]1)=[O:14])=O)C1C=CC=CC=1>[Pd]>[CH3:9][NH:11][CH2:12][C:13]([NH:15][CH:16]1[CH2:19][N:18]([C:20]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[O:21])[CH2:17]1)=[O:14]
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 58562550Tert-butyl 3-(2-(((benzyloxy)carbonyl)(methyl)amino)acetamido)azetidine-1-carboxylate

生成物 1

HCID 18699830Tert-butyl 3-(2-(methylamino)acetamido)azetidine-1-carboxylate

試薬・触媒・溶媒 1

HCID 23938Palladium触媒

実験手順

To a flask containing tert-butyl 3-(2-(((benzyloxy)carbonyl)(methyl)amino)acetamido)azetidine-1-carboxylate (3.10 g, 8.21 mmol, prepared in the previous step) and a stirbar, was added 10% Pd/C (136 g, 0.127 mmol). The flask was evacuated and back filled with argon. Methanol (100 mL) was carefully added via syringe and the flask was evacuated with stirring. It was then back filled with hydrogen and stirred 2 days under a hydrogen balloon. After evacuation with stirring and back filling with argon, the catalyst was removed by filtration over Celite 521 and concentrated in vacuo to afford the product.

後処理

  1. customprepared in the previous step) and a stirbar
  2. customThe flask was evacuated
  3. additionback filled with argon
  4. additionMethanol (100 mL) was carefully added via syringe
  5. customthe flask was evacuated
  6. additionIt was then back filled with hydrogen
  7. stirringstirred 2 days under a hydrogen balloon
  8. stirringAfter evacuation with stirring
  9. customthe catalyst was removed by filtration over Celite 521
  10. concentrationconcentrated in vacuo
  11. customto afford the product

出典と根拠

ORDレコード
ord-1ca087beb7a04993ad684d82397a94af
出典データセット
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08518969B2

反応ノート

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