1,4-Dioxane hydrochloride → (4-{[bis-(1H-imidazol-2-ylmethyl)-amino]-methyl}-phenyl)-piperazin-1-yl-methanone

HRID 348618노트

반응식

HRID 348618 반응식
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14](=[O:35])[C:15]2[CH:20]=[CH:19][C:18]([CH2:21][N:22]([CH2:29][C:30]3[NH:31][CH:32]=[CH:33][N:34]=3)[CH2:23][C:24]3[NH:25][CH:26]=[CH:27][N:28]=3)=[CH:17][CH:16]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.Cl.O1CCOCC1>CO>[NH:25]1[CH:26]=[CH:27][N:28]=[C:24]1[CH2:23][N:22]([CH2:21][C:18]1[CH:17]=[CH:16][C:15]([C:14]([N:11]2[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]2)=[O:35])=[CH:20][CH:19]=1)[CH2:29][C:30]1[NH:34][CH:33]=[CH:32][N:31]=1

참가 물질

4

반응물 2

HCID 204431481,4-Dioxane hydrochlorideHCID 66941477HCID 66941477, 화합물

생성물 1

HCID 21084462(4-{[bis-(1H-imidazol-2-ylmethyl)-amino]-methyl}-phenyl)-piperazin-1-yl-methanone수율 55.2%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

The compound (111 mg) obtained in Example 32-1 was dissolved in anhydrous methanol (1.0 ml) and then added with a 4 mol/l hydrogen chloride/dioxane solution (3.0 ml) and stirred at room temperature for 1 hour. After completion of the reaction, the solvent was distilled off and the residue was added with a 1 mol/l sodium hydroxide aqueous solution, followed by washing with dichloromethane. The aqueous layer was evaporated to dryness, followed by distilling azeotropically with chloroform. Consequently, the subject compound (48.5 mg) was obtained as a yellow oily substance.

후처리

  1. customAfter completion of the reaction
  2. distillationthe solvent was distilled off
  3. additionthe residue was added with a 1 mol/l sodium hydroxide aqueous solution
  4. washby washing with dichloromethane
  5. customThe aqueous layer was evaporated to dryness
  6. distillationby distilling azeotropically with chloroform

출처 및 근거

ORD 기록
ord-6997360aa9184de4aad00c2fdf04fea0
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07176227B2

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