Ammonium Chloride → 8-[3-(4-Diphenylmethylpiperazine-1-yl)-2-hydroxy-propoxy]isoquinoline

HRID 1195703ノート

反応式

HRID 1195703 の反応式
[OH:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[C:11]=1[CH:10]=[N:9][CH:8]=[CH:7]2.ClCC(O)C[CH:16]1[NH:21][CH2:20][CH2:19][N:18]([CH:22]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[CH2:17]1.[CH3:36][C:37](C)([O-:39])[CH3:38].[K+].[Cl-].[NH4+]>C1COCC1.C(Cl)Cl>[C:29]1([CH:22]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[N:18]2[CH2:17][CH2:16][N:21]([CH2:36][CH:37]([OH:39])[CH2:38][O:1][C:2]3[CH:3]=[CH:4][CH:5]=[C:6]4[C:11]=3[CH:10]=[N:9][CH:8]=[CH:7]4)[CH2:20][CH2:19]2)[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=1

参加物

7

反応物 4

HCID 25517Ammonium ChlorideHCID 23665647Potassium tert-butoxideHCID 867457733-(Chloro-2-hydroxypropyl)-1-diphenylmethylpiperazineHCID 1354417118-Hydroxyisoquinoline

生成物 1

HCID 200790268-[3-(4-Diphenylmethylpiperazine-1-yl)-2-hydroxy-propoxy]isoquinoline

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

In 15 ml of dried THF were dissolved 80 mg of 8-hydroxyisoquinoline and 204 mg of 4-(3-(chloro-2-hydroxypropyl)-1-diphenylmethylpiperazine synthesized in Example 23-(b), and 68 mg of potassium t-butoxide was further added thereto, followed by stirring at room temperature for 20 hours. The reaction liquid was then poured into 15 ml of an aqueous saturated ammonium chloride solution, and extraction was then performed with 150 ml of methylene chloride. After drying with an anhydrous Glauber's salt, the solvent was distilled off, and the resultant residue was purified through a silica gel thin-layer chromatograph. Development was carried out by the use of an effluent solvent of chloroform:methanol=25:1 for the purpose of separation and purification, with the result that 8-[3-(4-diphenylmethylpiperazine-1-yl)-2-hydroxy-propoxy]isoquinoline was obtained in an amount of 70 mg.

後処理

  1. additionwas further added
  2. customThe reaction liquid
  3. dry with materialAfter drying with an anhydrous Glauber's salt
  4. distillationthe solvent was distilled off
  5. customthe resultant residue was purified through a silica gel thin-layer chromatograph
  6. custommethanol=25:1 for the purpose of separation and purification

出典と根拠

ORDレコード
ord-2036fab978644b0683f23f3f01ace48f
出典データセット
uspto-grants-1992_05
特許番号
US05112817

反応ノート

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