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

HRID 490099
ノート
印刷プレビュー

反応式

HRID 490099 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 31275
1,4-Dioxane
溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-b9250beff4904051a0e31e6027b56d63
出典データセット
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07528132B2

反応ノート

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