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1-Phenylpiperazine → HCID 22762658、化合物

HRID 1112749
ノート
印刷プレビュー

反応式

HRID 1112749 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 22762658HCID 22762658、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.)

後処理

  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.

出典と根拠

ORDレコード
ord-01ba37137e7b4594b64869faa8f81677
出典データセット
uspto-grants-1978_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04123529

反応ノート

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