Triethylamine → 5-Methoxy-2-piperazin-1-yl-pyrimidine hydrochloride

HRID 84764

反応式

HRID 84764 の反応式
C(O[C:6]([N:8]1[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1)=O)(C)(C)C.[Cl:14]C1[N:20]=[CH:19][C:18]([O:21][CH3:22])=[CH:17][N:16]=1.C(N(CC)CC)C>CN(C=O)C>[ClH:14].[CH3:22][O:21][C:18]1[CH:17]=[N:16][C:6]([N:8]2[CH2:9][CH2:10][NH:11][CH2:12][CH2:13]2)=[N:20][CH:19]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 143452tert-Butyl piperazine-1-carboxylateHCID 5890582-Chloro-5-methoxypyrimidine

生成物 1

HCID 866866095-Methoxy-2-piperazin-1-yl-pyrimidine hydrochloride収率 51.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

1.5 g piperazine-1-carboxylic acid tert-butyl ester was added to 1.2 g 2-chlor-5-methoxy-pyrimidine and 2.2 mL triethylamine in 30 mL DMF. The reaction was stirred 6 days at 60° C. The solvent was removed and the residue was dissolved in dichlormethane and extracted with water. The organic layer was washed with a saturated sodiumchloride-solution and evaporated. The residue was purified by HPLC to give 957 mg desired product.

後処理

  1. customThe solvent was removed
  2. dissolutionthe residue was dissolved in dichlormethane
  3. extractionextracted with water
  4. washThe organic layer was washed with a saturated sodiumchloride-solution
  5. customevaporated
  6. customThe residue was purified by HPLC

出典と根拠

ORDレコード
ord-ead407df16ec434db4c7c75237acbeef
出典データセット
uspto-grants-2014_09
特許番号
US08846948B2

関連ノート

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