Hydrochloric Acid → 1-(o-Chlorophenoxy)-4-(4-phenyl-1-piperazinyl)-2-butanol

HRID 1463133

反応式

HRID 1463133 の反応式
[Cl:1][C:2]1[CH:14]=[CH:13][CH:12]=[CH:11][C:3]=1[O:4][CH:5](Cl)[CH:6]([OH:9])[CH2:7][CH3:8].[C:15]1([N:21]2[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]2)[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.Cl.[OH-].[Na+]>C(O)(C)C>[Cl:1][C:2]1[CH:14]=[CH:13][CH:12]=[CH:11][C:3]=1[O:4][CH2:5][CH:6]([OH:9])[CH2:7][CH2:8][N:24]1[CH2:25][CH2:26][N:21]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH2:22][CH2:23]1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 70961-PhenylpiperazineHCID 14798Sodium HydroxideHCID 198402391-(o-Chlorophenoxy)-2-hydroxybutyl chloride

生成物 1

HCID 131204511-(o-Chlorophenoxy)-4-(4-phenyl-1-piperazinyl)-2-butanol

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

A mixture of 35.1 g. (0.15 mole) of 1-(o-chlorophenoxy)-2-hydroxybutyl chloride, 32.6 g. (0.2 mole) of N-phenylpiperazine and 400 ml. of isopropanol was refluxed for 48 hr. The reaction mixture was allowed to stand in a refrigerator overnight and filtered. The filtrate was treated with ethereal hydrogen chloride and the salt precipitated by the addition of ether. The white crystalline solid which formed was dissolved in 0.1 mole of hydrochloric acid and then neutralized with sodium hydroxide producing a crystalline precipitate. This was recrystallized with isopropanol yielding 36 g. of the free base of the product which melted at 100°-101.5° C.

後処理

  1. additionA mixture of 35.1 g
  2. customto stand in a refrigerator overnight
  3. filtrationfiltered
  4. additionThe filtrate was treated with ethereal hydrogen chloride
  5. customthe salt precipitated by the addition of ether
  6. customThe white crystalline solid which formed
  7. customThis was recrystallized with isopropanol yielding 36 g

出典と根拠

ORDレコード
ord-af89ac321c3a4d74953eb2d540750729
出典データセット
uspto-grants-1984_07
特許番号
US04463190

関連ノート

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