Water → HCID 178523336, 화합물

HRID 1089122노트

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HRID 1089122 반응식
[OH:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][C:10]=2[OH:12])[N:5]=[CH:4][C:3]=1[C:13]([OH:15])=O.[C:16]1([CH:22]([C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)[N:23]2[CH2:28][CH2:27][N:26]([CH2:29][CH2:30][CH2:31][CH2:32][NH2:33])[CH2:25][CH2:24]2)[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.O>CS(C)=O>[C:34]1([CH:22]([C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=2)[N:23]2[CH2:24][CH2:25][N:26]([CH2:29][CH2:30][CH2:31][CH2:32][NH:33][C:13]([C:3]3[CH:4]=[N:5][C:6]4[C:11]([C:2]=3[OH:1])=[C:10]([OH:12])[CH:9]=[CH:8][CH:7]=4)=[O:15])[CH2:27][CH2:28]2)[CH:35]=[CH:36][CH:37]=[CH:38][CH:39]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 139569931-(4-Aminobutyl)-4-(diphenylmethyl)piperazineHCID 178524716HCID 178524716, 화합물

생성물 1

HCID 178523336HCID 178523336, 화합물수율 41.3%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

N,N'-Carbonyldiimidazole (1.2 g) is added to a solution of 4,5-dihydroxyquinoline-3-carboxylic acid (0.7 g), which is prepared according to the method described in Japanese Patent First Publication No. 65874/1981, in dry dimethyl sulfoxide (30 ml) and the mixture is stirred at room temperature for 30 minutes. 4-(4-Diphenylmethyl-1-piperazinyl)butylamine (2.2 g) is added to the reaction mixture and the mixture is stirred at room temperature for 6 hours, and thereto is added water (about 200 ml), and the mixture is extracted with chloroform. The organic layer is dried over anhydrous magnesium sulfate and the solvent is distilled off. The residue is subjected to silica gel column chromatography, followed by elution with chloroform - methanol (30 : 1). The obtained crystals are recrystallized from isopropyl alcohol to give the desired compound (0.72 g). m.p. 215° to 218° C.

후처리

  1. customis prepared
  2. extractionthe mixture is extracted with chloroform
  3. dry with materialThe organic layer is dried over anhydrous magnesium sulfate
  4. distillationthe solvent is distilled off
  5. washfollowed by elution with chloroform - methanol (30 : 1)
  6. customThe obtained crystals are recrystallized from isopropyl alcohol

출처 및 근거

ORD 기록
ord-a142bd64f53347f9ab9ce5ff40d1c648
출처 데이터셋
uspto-grants-1990_10
특허 번호
US04965266

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