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

HRID 64701

반응식

HRID 64701 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a63c9a72ac364cb3ad8467f039c0d8f8
출처 데이터셋
uspto-grants-1986_09
특허 번호
US04609735

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