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Benzyl 3-[(4-cyclobutylpiperazin-1-yl)carbonyl]azetidine-1-carboxylate → 1-(Azetidin-3-ylcarbonyl)-4-cyclobutylpiperazine

HRID 1402762
ノート
印刷プレビュー

反応式

HRID 1402762 の反応式
[CH:1]1([N:5]2[CH2:10][CH2:9][N:8]([C:11]([CH:13]3[CH2:16][N:15](C(OCC4C=CC=CC=4)=O)[CH2:14]3)=[O:12])[CH2:7][CH2:6]2)[CH2:4][CH2:3][CH2:2]1>CCO.[Pd]>[NH:15]1[CH2:14][CH:13]([C:11]([N:8]2[CH2:9][CH2:10][N:5]([CH:1]3[CH2:2][CH2:3][CH2:4]3)[CH2:6][CH2:7]2)=[O:12])[CH2:16]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 66739735Benzyl 3-[(4-cyclobutylpiperazin-1-yl)carbonyl]azetidine-1-carboxylate

生成物 1

HCID 667393151-(Azetidin-3-ylcarbonyl)-4-cyclobutylpiperazine収率 74.6%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

To a stirred solution of benzyl 3-[(4-cyclobutylpiperazin-1-yl)carbonyl]azetidine-1-carboxylate (130 mg, 0.36 mmol) in EtOH (10 mL) was added 10% Pd/C (13 mg, 10% wt/wt). The flask was evacuated and the vacuum purged with N2 gas. The flask was evacuated again and the vacuum purged with H2 gas. After 16 hours the reaction mixture was filtered through Celite® and charged with 10% Pd/C (13 mg, 10% wt/wt). The flask was evacuated and the vacuum purged with N2 gas. The flask was evacuated again and the vacuum purged with H2 gas. After 23 hours, the reaction mixture was filtered through Celite® and the filtrate concentrated at reduced pressure to give the final compound (60 mg, 74%) which was used without further purification.

後処理

  1. customThe flask was evacuated
  2. customthe vacuum purged with N2 gas
  3. customThe flask was evacuated again
  4. customthe vacuum purged with H2 gas
  5. filtrationAfter 16 hours the reaction mixture was filtered through Celite®
  6. additioncharged with 10% Pd/C (13 mg, 10% wt/wt)
  7. customThe flask was evacuated
  8. customthe vacuum purged with N2 gas
  9. customThe flask was evacuated again
  10. customthe vacuum purged with H2 gas
  11. filtrationthe reaction mixture was filtered through Celite®
  12. concentrationthe filtrate concentrated at reduced pressure

出典と根拠

ORDレコード
ord-006811dfd83144d2a5bc891c8af923eb
出典データセット
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08912176B2

反応ノート

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