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

HRID 84764

반응식

HRID 84764 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 866866095-Methoxy-2-piperazin-1-yl-pyrimidine hydrochloride수율 51.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
60 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ead407df16ec434db4c7c75237acbeef
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846948B2

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