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Piperazine → HCID 22349876, 화합물

HRID 896218
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HRID 896218 반응식
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.[C:7]([C:11]1[N:16]=[C:15](Cl)[CH:14]=[C:13]([CH:18]([F:20])[F:19])[N:12]=1)([CH3:10])([CH3:9])[CH3:8]>C(O)C>[C:7]([C:11]1[N:16]=[C:15]([N:1]2[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]2)[CH:14]=[C:13]([CH:18]([F:19])[F:20])[N:12]=1)([CH3:10])([CH3:8])[CH3:9]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 4837PiperazineHCID 22349860HCID 22349860, 화합물

생성물 1

HCID 22349876HCID 22349876, 화합물수율 82.4%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
78 °C

실험 절차

6.3 g of piperazine (73.5 mmol) were dissolved in 50 ml of ethanol. 2.31 g of 2-tert-butyl-4-chloro-6-difluoromethyl-pyrimidine (10.5 mmol) were added and the mixture was stirred for 3 h at 78° C. The solvent was evaporated and the residue was added slowly to 100 ml of water. After cooling, the pH was adjusted to 12 with 2 N aqueous sodium hydroxide, and aqueos layer was extracted with dichloromethane. The organic layer was dried over magnesium sulfate, filtered and the solvent was evaporated to yield 2.34 g of the title compound.

후처리

  1. customThe solvent was evaporated
  2. additionthe residue was added slowly to 100 ml of water
  3. temperatureAfter cooling
  4. extractionwas extracted with dichloromethane
  5. dry with materialThe organic layer was dried over magnesium sulfate
  6. filtrationfiltered
  7. customthe solvent was evaporated

출처 및 근거

ORD 기록
ord-6cd42610f81f4a068a02be886b534a00
출처 데이터셋
uspto-grants-2005_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06919342B2

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