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4,6-Dichloropyrimidine → 4-Chloro-6-(piperazin-1-yl)pyrimidine

HRID 68556
ノート
印刷プレビュー

反応式

HRID 68556 の反応式
[N:1]1([C:7](OC(C)(C)C)=O)[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.CCN(C(C)C)C(C)C.[Cl:23][C:24]1[CH:29]=C(Cl)[N:27]=[CH:26][N:25]=1>ClCCl>[Cl:23][C:24]1[CH:29]=[C:7]([N:1]2[CH2:2][CH2:3][NH:4][CH2:5][CH2:6]2)[N:27]=[CH:26][N:25]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 709434,6-DichloropyrimidineHCID 81531DiisopropylethylamineHCID 143452tert-Butyl piperazine-1-carboxylate

生成物 1

HCID 160922664-Chloro-6-(piperazin-1-yl)pyrimidine収率 98%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

13.3 g tert-butyl 1-piperazinecarboxylate and 11.2 mL DIPEA were added to 10 g 4, 6 dichloro pyrimidine in 1000 mL dichlormethane was stirred over the weekend at RT. The solvent was removed. The residue was dissolved in 200 mL dichlormethane and 200 mL trifluoro acetic acid was added. The reaction was stirred at RT. The solvent was removed. The residue was dissolved in methanol and passed through HCO3 containing resin. The solvent was removed and the residue was purified by chromatographie on silica (dcyclohexane: ethylacetate 0-40%) to yield 13.07 g of the desired product.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. customThe solvent was removed
  2. dissolutionThe residue was dissolved in 200 mL dichlormethane
  3. addition200 mL trifluoro acetic acid was added
  4. stirringThe reaction was stirred at RT
  5. customThe solvent was removed
  6. dissolutionThe residue was dissolved in methanol
  7. customThe solvent was removed
  8. customthe residue was purified by chromatographie on silica (dcyclohexane: ethylacetate 0-40%)

出典と根拠

ORDレコード
ord-fcc9c374f65c4aafa624fd70903d5b38
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08822464B2

反応ノート

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