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

HRID 2247844ノート

反応式

HRID 2247844 の反応式
[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

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 3776IsopropanolHCID 915212-((1-Naphthalenyloxy)methyl)oxiraneHCID 14966308HCID 14966308、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-82f7cfa5078c448494299f8eb40bc5d3
出典データセット
uspto-grants-1991_08
特許番号
US05037828

反応ノート

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