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

HRID 543185ノート

反応式

HRID 543185 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3a64204a83624edcb2c79cd26f705bd5
出典データセット
uspto-grants-1987_04
特許番号
US04661481

反応ノート

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