Triethylamine → 2-Bromo-1-(4-pyrimidin-2-ylpiperazin-1-yl)ethanone

HRID 68553

反応式

HRID 68553 の反応式
[Br:1][CH2:2][C:3](Br)=[O:4].[N:6]1[CH:11]=[CH:10][CH:9]=[N:8][C:7]=1[N:12]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1.C(N(CC)CC)C>C1COCC1>[Br:1][CH2:2][C:3]([N:15]1[CH2:16][CH2:17][N:12]([C:7]2[N:6]=[CH:11][CH:10]=[CH:9][N:8]=2)[CH2:13][CH2:14]1)=[O:4]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 61147Bromoacetyl bromideHCID 887471-(2-Pyrimidinyl)piperazine

生成物 1

HCID 636798462-Bromo-1-(4-pyrimidin-2-ylpiperazin-1-yl)ethanone収率 0.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

20.2 g bromacetylbromide was dropped to 16.5 g 1-pyrimidin-2-yl-piperazin and 10.2 g triethylamine in 250 mL THF. The reaction was stirred over night at RT and evaporated. The residue was extracted with DCM and water. The organic layer was evaporated and the residue was crystallized with petrolether and then purified by chromatography on silica gel (DCM/MeOH:95/5) to yield 36 mg of the desired compound.

後処理

  1. customevaporated
  2. extractionThe residue was extracted with DCM and water
  3. customThe organic layer was evaporated
  4. customthe residue was crystallized with petrolether
  5. custompurified by chromatography on silica gel (DCM/MeOH:95/5)

出典と根拠

ORDレコード
ord-f971d6ac5dfa4b12a4f4c5f44ffe44c2
出典データセット
uspto-grants-2014_09
特許番号
US08822464B2

関連ノート

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