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Ethyl Acetate → 5-(4-Boc-piperazin-1-yl)-3-chloro[1,2,4]triazine

HRID 490099
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HRID 490099 반응식
[Cl:1][C:2]1[N:3]=[N:4][CH:5]=[C:6](Cl)[N:7]=1.C(N(C(C)C)CC)(C)C.[C:18]([N:25]1[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]1)([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19].C(OCC)(=O)C>O1CCOCC1>[C:18]([N:25]1[CH2:26][CH2:27][N:28]([C:6]2[N:7]=[C:2]([Cl:1])[N:3]=[N:4][CH:5]=2)[CH2:29][CH2:30]1)([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19]
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참가 물질

6

반응물 4

HCID 8857Ethyl AcetateHCID 81531DiisopropylethylamineHCID 143452tert-Butyl piperazine-1-carboxylateHCID 122649333,5-Dichloro-1,2,4-triazine

생성물 1

HCID 576741865-(4-Boc-piperazin-1-yl)-3-chloro[1,2,4]triazine수율 31.1%

시약·촉매·용매 1

HCID 31275
1,4-Dioxane
용매

실험 절차

To a solution of 3,5-dichloro[1,2,4]triazine (0.34 g, 2.28 mmol.) in anhydrous dioxane (4 mL) was add diisopropylethylamine (0.44 g, 3.41 mmol.) and N—Boc-piperazine (0.424 g, 2.28 mmol.). The reaction mixture was stirred at room temperature for 40 minutes. Ethyl acetate (200 mL) was added. The organic solution was washed with saturated ammonium chloride solution, water and brine. The organic layer was dried over sodium sulfate. The organic solvent was evaporation under reduced pressure. The crude product was purified by RP-HPLC to yield the desired 5-(4-Boc-piperazin-1-yl)-3-chloro[1,2,4]triazine 151 (0.212 g, 0.71 mmol.).

후처리

  1. washThe organic solution was washed with saturated ammonium chloride solution, water and brine
  2. dry with materialThe organic layer was dried over sodium sulfate
  3. customevaporation under reduced pressure
  4. customThe crude product was purified by RP-HPLC

출처 및 근거

ORD 기록
ord-b9250beff4904051a0e31e6027b56d63
출처 데이터셋
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07528132B2

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