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Acetyl chloride → Tert-butyl 4-acetylpiperazine-1-carboxylate

HRID 1257108
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HRID 1257108 반응식
[C:1]([N:8]1[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].C(N(CC)CC)C.[C:21](Cl)(=[O:23])[CH3:22]>ClCCl>[C:21]([N:11]1[CH2:10][CH2:9][N:8]([C:1]([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2])[CH2:13][CH2:12]1)(=[O:23])[CH3:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 143452tert-Butyl piperazine-1-carboxylate

생성물 1

HCID 22707023Tert-butyl 4-acetylpiperazine-1-carboxylate수율 85%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of N-Boc-piperazine (300 mg, 1.63 mmol), triethylamine (494 mg, 3 equiv), and acetyl chloride (1.5 equiv) in dichloromethane was stirred overnight at rt. The solution was quenched by the dropwise addition of water. The organic layer was separated, dried over anhydrous Na2SO4, and evaporated in vacuo. The residue was purified by flash chromatography to give the title compound (˜85% yield) as a solid.

후처리

  1. customThe solution was quenched by the dropwise addition of water
  2. customThe organic layer was separated
  3. dry with materialdried over anhydrous Na2SO4
  4. customevaporated in vacuo
  5. customThe residue was purified by flash chromatography

출처 및 근거

ORD 기록
ord-17373938cac64b8cac4b38ed704fe09c
출처 데이터셋
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08461339B2

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