1-(2-Methoxyphenyl)-4-(1-(4-phenylphenyl)cyclohex-1-en-4-yl)piperazine → HCID 178489564, 화합물

HRID 54202노트

반응식

HRID 54202 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH2:14][CH2:13][N:12]([CH:15]2[CH2:20][CH2:19][C:18]([C:21]3[CH:26]=[CH:25][C:24]([C:27]4[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=4)=[CH:23][CH:22]=3)=[CH:17][CH2:16]2)[CH2:11][CH2:10]1>C(O)(=O)C.[Pd]>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH2:10][CH2:11][N:12]([C@H:15]2[CH2:20][CH2:19][C@H:18]([C:21]3[CH:22]=[CH:23][C:24]([C:27]4[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=4)=[CH:25][CH:26]=3)[CH2:17][CH2:16]2)[CH2:13][CH2:14]1

참가 물질

4

반응물 1

HCID 199585511-(2-Methoxyphenyl)-4-(1-(4-phenylphenyl)cyclohex-1-en-4-yl)piperazine

생성물 1

HCID 178489564HCID 178489564, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 176Acetic Acid용매

실험 절차

1-(2-Methoxyphenyl)-4-(1-(4-phenylphenyl)cyclohex-1-en-4-yl)piperazine (2.7 g, 5.4 mmol) was hydrogenated at 50 psi (about 3.5×105N.m-2) above atmospheric pressure at 45° C. in acetic acid (50 ml), using 10% Pd/C (2.4 g) as a catalyst for three days. The volatiles were evaporated in vacuo and the residue was partitioned between dichloromethane (150 ml) and sat. NaHCO3 (200 ml). The organic layer was separated and washed with brine and evaporated in vacuo. The residues were recrystallised from dichloromethane and again from methanol. The white solid was dissolved in ether and acidified to pH 1 with ethereal HCl. The volatiles were removed in vacuo to give the title compound as the one and a half hydrochloride; three quarters hydrate (0.281 g), m.p. 220°-225° C.

후처리

  1. customfor three days
  2. customThe volatiles were evaporated in vacuo
  3. customthe residue was partitioned between dichloromethane (150 ml) and sat. NaHCO3 (200 ml)
  4. customThe organic layer was separated
  5. washwashed with brine
  6. customevaporated in vacuo
  7. customThe residues were recrystallised from dichloromethane and again from methanol
  8. dissolutionThe white solid was dissolved in ether
  9. customThe volatiles were removed in vacuo

출처 및 근거

ORD 기록
ord-d55d7cc28e1a48f58fe03a4724d0e591
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05622951

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