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

HRID 543187
ノート
印刷プレビュー

反応式

HRID 543187 の反応式
[N:1]1([CH2:7][CH2:8][CH2:9][NH:10][C:11]([NH:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19])=[O:12])[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.[F:20][C:21]([F:32])([F:31])[C:22]1[CH:23]=[C:24]([CH:27]=[CH:28][C:29]=1[Cl:30])[CH2:25][Cl:26].C(N(CC)CC)C>C(O)C>[ClH:26].[ClH:26].[F:31][C:21]([F:20])([F:32])[C:22]1[CH:23]=[C:24]([CH:27]=[CH:28][C:29]=1[Cl:30])[CH2:25][N:4]1[CH2:3][CH2:2][N:1]([CH2:7][CH2:8][CH2:9][NH:10][C:11]([NH:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19])=[O:12])[CH2:6][CH2:5]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 130942621-Chloro-4-(chloromethyl)-2-(trifluoromethyl)benzeneHCID 571432471-(3-Piperazinylpropyl)-3-n-hexylurea

生成物 1

HCID 136067271-{3-[4-(3-Trifluoromethyl-4-chlorobenzyl)piperazin-1-yl]propyl}-3-n-hexylurea dihydrochloride収率 115.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 1-(3-piperazinylpropyl)-3-n-hexylurea (2.7 g; 10 mmole), 3-trifluoromethyl-4-chloro-benzyl chloride (2.29 g; 10 mmole), triethylamine (1.01 g; 10 mmole) and ethanol (30 ml) was refluxed for 3 hours. The solvent was evaporated in vacuo, and water was added to the residue. The product was extracted with ether, and the extract was dried (sodium sulfate) and concentrated. Precipitation of the oily residue with ethereal hydrochloric acid, followed by recrystallization from alcohol, provided the title compound (3.1 g; 58% yield) as colorless crystals, m.p. 216°-219° C.

後処理

  1. temperaturewas refluxed for 3 hours
  2. customThe solvent was evaporated in vacuo, and water
  3. additionwas added to the residue
  4. extractionThe product was extracted with ether
  5. dry with materialthe extract was dried (sodium sulfate)
  6. concentrationconcentrated
  7. customPrecipitation of the oily residue with ethereal hydrochloric acid
  8. customfollowed by recrystallization from alcohol

出典と根拠

ORDレコード
ord-ec5e8acdc7ad4825a7617784dd8cf890
出典データセット
uspto-grants-1987_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04661481

反応ノート

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