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1-Phenylpiperazine → HCID 22762658, 화합물

HRID 1112749
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HRID 1112749 반응식
Cl.[CH2:2]([C:5]1[S:6][CH:7]=[C:8]([CH2:10]Cl)[N:9]=1)[CH2:3][CH3:4].[C:12]1([N:18]2[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]2)[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.C(=O)([O-])[O-].[Na+].[Na+]>C(O)C>[CH2:2]([C:5]1[S:6][CH:7]=[C:8]([CH2:10][N:21]2[CH2:22][CH2:23][N:18]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[CH2:19][CH2:20]2)[N:9]=1)[CH2:3][CH3:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 70961-PhenylpiperazineHCID 10340Sodium CarbonateHCID 2276262765386-29-0

생성물 1

HCID 22762658HCID 22762658, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 2-n-propyl-4-chloromethylthiazole hydrochloride (3.18g; 0.015 mole), 1-phenylpiperazine (2.43g; 0.015 mole) and sodium carbonate (anhydrous, 10g) in absolute ethanol (60ml) was stirred and boiled under reflux for 6 hours. The suspension was filtered and the filtrate evaporated to a yellow oil. This was dissolved in boiling benzene and treated with decolourising charcoal. After filtration, the benzene was removed giving a yellow oil which crystallised 4.27g. This solid was recrystallised from petroleum ether (b.p. 60°-80° C.) at 0° C. to give a white crystalline solid (m.p. 38°-39° C.)

후처리

  1. temperatureunder reflux for 6 hours
  2. filtrationThe suspension was filtered
  3. customthe filtrate evaporated to a yellow oil
  4. dissolutionThis was dissolved
  5. additiontreated with decolourising charcoal
  6. filtrationAfter filtration
  7. customthe benzene was removed
  8. customgiving a yellow oil which
  9. customcrystallised 4.27g
  10. customThis solid was recrystallised from petroleum ether (b.p. 60°-80° C.) at 0° C.

출처 및 근거

ORD 기록
ord-01ba37137e7b4594b64869faa8f81677
출처 데이터셋
uspto-grants-1978_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04123529

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