Triethylamine → 1-{3-[4-[3-(4-Chlorophenyl)propyl]piperazin-1-yl]-propyl}-3-n-hexylurea dihydrochloride

HRID 1380198노트

반응식

HRID 1380198 반응식
[Cl:1][CH2:2][CH2:3][CH2:4][NH:5][C:6]([NH:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14])=[O:7].[Cl:15][C:16]1[CH:21]=[CH:20][C:19]([CH2:22][CH2:23][CH2:24][N:25]2[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]2)=[CH:18][CH:17]=1.C(N(CC)CC)C>CCOCC>[ClH:1].[ClH:15].[Cl:15][C:16]1[CH:21]=[CH:20][C:19]([CH2:22][CH2:23][CH2:24][N:25]2[CH2:26][CH2:27][N:28]([CH2:2][CH2:3][CH2:4][NH:5][C:6]([NH:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14])=[O:7])[CH2:29][CH2:30]2)=[CH:18][CH:17]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 1628731-(3-(4-Chlorophenyl)propyl)piperazineHCID 136067321-(3-Chloropropyl)-3-n-hexylurea

생성물 1

HCID 136067251-{3-[4-[3-(4-Chlorophenyl)propyl]piperazin-1-yl]-propyl}-3-n-hexylurea dihydrochloride수율 64.5%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

A mixture of 1-(3-chloropropyl)-3-n-hexylurea (2.21 g; 10 mmole), 1-[3-(4-chlorophenyl)propyl]piperazine (2.39 g; 10 mmole), triethylamine (1.01 g; 10 mmole) and alcohol (25 ml) was refluxed for 18 hours. The cooled reaction mixture was diluted with ether and washed with water, dried (sodium sulfate) and concentrated in vacuo. The resulting yellow viscous oil was purified on a silica gel column (methylene chloride/methanol; 93:7) and precipitated with ethereal hydrochloric acid to provide the title compound (1.6 g; 38% yield) as colorless crystals, m.p. 213°-216° C.

후처리

  1. temperaturewas refluxed for 18 hours
  2. customThe cooled reaction mixture
  3. washwashed with water
  4. dry with materialdried (sodium sulfate)
  5. concentrationconcentrated in vacuo
  6. customThe resulting yellow viscous oil was purified on a silica gel column (methylene chloride/methanol; 93:7)
  7. customprecipitated with ethereal hydrochloric acid

출처 및 근거

ORD 기록
ord-f311854efdbd49e0a98586968b38e346
출처 데이터셋
uspto-grants-1986_04
특허 번호
US04579947

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