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

HRID 1402762
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HRID 1402762 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

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

생성물 1

HCID 667393151-(Azetidin-3-ylcarbonyl)-4-cyclobutylpiperazine수율 74.6%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-006811dfd83144d2a5bc891c8af923eb
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08912176B2

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