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Sodium Chloride → 4-(tert-Butoxycarbonyl)-2,2-dimethyl-1-[4-(pyridin-4-yl)benzoyl]piperazine

HRID 352830
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HRID 352830 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][NH:11][C:10]([CH3:15])([CH3:14])[CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[N:16]1[CH:21]=[CH:20][C:19]([C:22]2[CH:30]=[CH:29][C:25]([C:26]([O-])=[O:27])=[CH:24][CH:23]=2)=[CH:18][CH:17]=1.[Cl-].[Na+]>CN(C)C=O.C(N(CC)CC)C.C(Cl)Cl>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:26](=[O:27])[C:25]2[CH:24]=[CH:23][C:22]([C:19]3[CH:18]=[CH:17][N:16]=[CH:21][CH:20]=3)=[CH:30][CH:29]=2)[C:10]([CH3:15])([CH3:14])[CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
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참가 물질

7

반응물 3

HCID 5234Sodium ChlorideHCID 227103871-Boc-3,3-dimethylpiperazineHCID 227111444-(4-Pyridyl)benzoate

생성물 1

HCID 227107644-(tert-Butoxycarbonyl)-2,2-dimethyl-1-[4-(pyridin-4-yl)benzoyl]piperazine

시약·촉매·용매 3

HCID 6228Dimethylformamide용매HCID 6344
Dichloromethane
용매
HCID 8471Triethylamine용매

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온도
60 °C

실험 절차

To a solution of 1-(tert-butoxycarbonyl)-3,3-dimethylpiperazine (173 mg) in a mixture of N,N-dimethylformamide (2.5 ml) and triethylamine (1.0 ml) was added (4-nirophenyl) 4-(4-pyridyl)benzoate (330 mg). The resulting mixture was stirred at 60° C. for 5 days. The reaction mixture was diluted with methylene chloride and then added with a saturated aqueous solution of sodium chloride to form two layers. The organic layer obtained by separation was washed with a saturated aqueous solution of sodium bicarbonate and an aqueous solution of sodium chloride, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The crudely purified product was purified by chromatography on a silica gel column (methylene chloride:methanol=50:1), whereby the title compound (199 mg) was obtained as colorless amorphous.

후처리

  1. customto form two layers
  2. customThe organic layer obtained by separation
  3. washwas washed with a saturated aqueous solution of sodium bicarbonate
  4. dry with materialan aqueous solution of sodium chloride, dried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe crudely purified product was purified by chromatography on a silica gel column (methylene chloride:methanol=50:1), whereby the title compound (199 mg)
  7. customwas obtained as colorless amorphous

출처 및 근거

ORD 기록
ord-275e5b49534645a393c00e5c79668fb3
출처 데이터셋
uspto-grants-2004_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06747023B1

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