Hydrochloric Acid → 4-(4-{2-Hydroxy-3-[(naphthalen-1-yl)oxy]propyl}piperazin-1-yl)-3-methoxyphenol

HRID 2247844노트

반응식

HRID 2247844 반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([OH:9])[CH:6]=[CH:5][C:4]=1[N:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1.[C:16]1([O:26][CH2:27][CH:28]2[O:30][CH2:29]2)[C:25]2[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=2)[CH:19]=[CH:18][CH:17]=1.C(O)(C)C.Cl>CO.C(OCC)C>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([OH:9])[CH:6]=[CH:5][C:4]=1[N:10]1[CH2:15][CH2:14][N:13]([CH2:29][CH:28]([OH:30])[CH2:27][O:26][C:16]2[C:25]3[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=3)[CH:19]=[CH:18][CH:17]=2)[CH2:12][CH2:11]1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 3776IsopropanolHCID 915212-((1-Naphthalenyloxy)methyl)oxiraneHCID 14966308HCID 14966308, 화합물

생성물 1

HCID 1314914-(4-{2-Hydroxy-3-[(naphthalen-1-yl)oxy]propyl}piperazin-1-yl)-3-methoxyphenol

시약·촉매·용매 2

HCID 887Methanol용매HCID 3283Diethyl Ether용매

실험 절차

A solution of 4.16 g. (0.02 mole) 1-(2-methoxy-4-hydroxyphenyl)-piperazine and 4.2 g. (0.021 mole) 2,3-epoxypropyl naphthyl ether in 50 ml. isopropanol is heated under reflux for 4 hours, while stirring. The solution is evaporated and the tarry residue obtained is dissolved in methanol. It is acidified with isopropanolic hydrochloric acid and diethyl ether carefully added thereto, an oily product precipitating out which is separated by decanting off. The solution is diluted with acetone. After a short time, the compound begins to crystallise out. When crystallisation is complete, the crystals are filtered off with suction and again recrystallised from methanol/diethyl either. Yield 4.8 g. (50% of theory); m.p. 230°-232° C.

후처리

  1. temperatureunder reflux for 4 hours
  2. customThe solution is evaporated
  3. customthe tarry residue obtained
  4. additioncarefully added
  5. customan oily product precipitating out which
  6. customis separated
  7. customby decanting off
  8. additionThe solution is diluted with acetone
  9. customto crystallise out
  10. customWhen crystallisation
  11. filtrationthe crystals are filtered off with suction
  12. customagain recrystallised from methanol/diethyl either

출처 및 근거

ORD 기록
ord-82f7cfa5078c448494299f8eb40bc5d3
출처 데이터셋
uspto-grants-1991_08
특허 번호
US05037828

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