Triethylamine → N-[2-[4-(2-Pyrimidinyl)-1-piperazinyl]ethyl]-2-benzofurancarboxamide Dihydrochloride Hydrate

HRID 374794

반응식

HRID 374794 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[N:3][C:2]=1[N:7]1[CH2:12][CH2:11][N:10]([CH2:13][CH2:14][NH2:15])[CH2:9][CH2:8]1.[O:16]1[C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=2[CH:18]=[C:17]1[C:25]([Cl:27])=[O:26].C(N(CC)CC)C>C(Cl)Cl>[OH2:16].[ClH:27].[ClH:27].[N:1]1[CH:6]=[CH:5][CH:4]=[N:3][C:2]=1[N:7]1[CH2:12][CH2:11][N:10]([CH2:13][CH2:14][NH:15][C:25]([C:17]2[O:16][C:20]3[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=3[CH:18]=2)=[O:26])[CH2:9][CH2:8]1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 389492-Benzofurancarbonyl chlorideHCID 138853581-Piperazineethanamine, 4-(2-pyrimidinyl)-

생성물 1

HCID 18995774N-[2-[4-(2-Pyrimidinyl)-1-piperazinyl]ethyl]-2-benzofurancarboxamide Dihydrochloride Hydrate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a stirred solution of [4-(2-pyrimidinyl)piperazinyl]ethylamine (2.0.g, 0.01 mol) in 50 mL of methylene chloride, benzofurane-2-carboxylic acid chloride (2.6 g, 0.014 mol) and triethylamine (2 g, 0.02 mol) were added. Stirring was continued at room temperature overnight. The methylene chloride solution was washed with water, dried over anhydrous sodium sulfate and evaporated under reduced pressure. The remaining residue was subjected to preparative HPLC. The title compound was separated and converted to the dihydrochloride hydrate salt with ethanolic HCl (0.5 g), m.p. 193° C.

후처리

  1. washThe methylene chloride solution was washed with water
  2. dry with materialdried over anhydrous sodium sulfate
  3. customevaporated under reduced pressure
  4. customThe title compound was separated

출처 및 근거

ORD 기록
ord-437e36131a6f42fc8dbc1160de94b4ac
출처 데이터셋
uspto-grants-1996_01
특허 번호
US05482940

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