Potassium Carbonate → HCID 14726460, 화합물

HRID 1087158노트

반응식

HRID 1087158 반응식
[Cl:1][C:2]1[N:3]=[N:4][C:5]([Cl:9])=[CH:6][C:7]=1Cl.C(=O)([O-])[O-].[K+].[K+].[NH2:16][CH2:17][CH2:18][CH2:19][CH2:20][N:21]1[CH2:26][CH2:25][N:24]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=2[O:33][CH3:34])[CH2:23][CH2:22]1>C(#N)C>[Cl:1][C:2]1[N:3]=[N:4][C:5]([Cl:9])=[CH:6][C:7]=1[NH:16][CH2:17][CH2:18][CH2:19][CH2:20][N:21]1[CH2:26][CH2:25][N:24]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=2[O:33][CH3:34])[CH2:23][CH2:22]1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 951233,4,6-TrichloropyridazineHCID 109999031-(4-Aminobutyl)-4-(2-methoxyphenyl)piperazine

생성물 1

HCID 14726460HCID 14726460, 화합물수율 54.2%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

9.25 g (0.050 mol) of 3,4,6-trichloropyridazine are stirred with 6.90 g (0.050 mol) of powdered anhydrous potassium carbonate and 13.15 g (0.050 mol) of 1-(4-aminobutyl)-4-(2-methoxyphenyl)piperazine in 1350 ml of dry acetonitrile at room temperature for 96 hours. The mixture is subsequently filtered with suction, and the filtrate is concentrated in vacuo. The residue is taken up in ethanol, and the trihydrochloride of 3,6-dichloro-4-((4-(4-(2-methoxyphenyl)-1-piperazinyl)butyl)amino)pyridazine of m.p.: 155°-170° C. is precipitated with ethereal HCl; yield: 54.2% of theory.

후처리

  1. filtrationThe mixture is subsequently filtered with suction
  2. concentrationthe filtrate is concentrated in vacuo
  3. customthe trihydrochloride of 3,6-dichloro-4-((4-(4-(2-methoxyphenyl)-1-piperazinyl)butyl)amino)pyridazine of m.p.: 155°-170° C. is precipitated with ethereal HCl

출처 및 근거

ORD 기록
ord-e2ecf7f680624a02b4740b552ea00331
출처 데이터셋
uspto-grants-1991_07
특허 번호
US05034391

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