Hydrochloric Acid → HCID 136359214, 화합물

HRID 1153959

반응식

HRID 1153959 반응식
C(=O)([O-])[O-].[K+].[K+].[Cl:7]C1C=C(N2CCN(C[CH2:21][CH2:22][N:23]3[C:27](=[O:28])[N:26]=[C:25](CC)[NH:24]3)CC2)C=CC=1.[O:31](CCBr)[C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1.[I-].[K+].ClC1C=C(N2CCN(CCCN3C(=O)N(CCOC4C=CC=CC=4)C(CC)=N3)CC2)C=CC=1.Cl>C(#N)C.C(O)C>[ClH:7].[O:31]([CH2:21][CH2:22][N:23]1[C:27](=[O:28])[NH:26][CH:25]=[N:24]1)[C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1

참가 물질

9

반응물 6

HCID 313Hydrochloric AcidHCID 4449NefazodoneHCID 4875Potassium IodideHCID 11430Potassium Carbonate2회HCID 68526Benzene, (2-bromoethoxy)-HCID 178437794HCID 178437794, 화합물

생성물 1

HCID 136359214HCID 136359214, 화합물수율 53%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 6342Acetonitrile용매2회

실험 절차

Reaction in Acetonitrile With Potassium Carbonate. A mixture of 2-[3-[4-(3-chlorophenyl)-1-piperazinyl]propyl]-5-ethyl-1H-1,2,4-triazol-3(2H)-one (15 g., 0.043 mole), phenoxyethyl bromide (8.62 g., 0.043 mole), potassium carbonate (11.9 g., 0.086 mole) and a trace of potassium iodide in 100 ml. of acetonitrile is refluxed for a 64 hr. period. The reaction mixture is filtered, the filtrate concentrated under reduced pressure and residual material taken up in ether and filtered. Concentration of the ethereal filtrate affords 18.35 g. (91%) of the free base product 2-[3-[4-(3-chlorophenyl)-1-piperazinyl]propyl]-5-ethyl-4-(2-phenoxyethyl)-2H-1,2,4-triazol-3(4h)-one. The free base is converted to the hydrochloride in ethanol employing ethanolic hydrogenchloride and crystallized from ethanol to afford a 53% yield of analytically pure 2-[3-[4-(3-chlorophenyl)-1-piperazinyl]propyl]-5-ethyl-4-(2 -phenoxyethyl-2H-1,2,4-triazol-3(4H)-one hydrochloride, m.p. 175°-177° C.

후처리

  1. filtrationThe reaction mixture is filtered
  2. concentrationthe filtrate concentrated under reduced pressure and residual material
  3. filtrationfiltered
  4. customConcentration of the ethereal filtrate affords 18.35 g
  5. customcrystallized from ethanol

출처 및 근거

ORD 기록
ord-c3c42eef760742febe035aae7ba031d4
출처 데이터셋
uspto-grants-1984_12
특허 번호
US04487773

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