Ethanol → 3-[4-(4-Chlorobenzyl)homopiperazin-1-yl]-propanethiol

HRID 2290900

反応式

HRID 2290900 の反応式
NC(N)=[S:3].[Cl:5][C:6]1[CH:23]=[CH:22][C:9]([CH2:10][N:11]2[CH2:17][CH2:16][CH2:15][N:14]([CH2:18][CH2:19][CH2:20]Cl)[CH2:13][CH2:12]2)=[CH:8][CH:7]=1.C(O)C.[OH-].[Na+]>O>[Cl:5][C:6]1[CH:23]=[CH:22][C:9]([CH2:10][N:11]2[CH2:17][CH2:16][CH2:15][N:14]([CH2:18][CH2:19][CH2:20][SH:3])[CH2:13][CH2:12]2)=[CH:8][CH:7]=1

参加物

6

反応物 4

HCID 702EthanolHCID 14798Sodium HydroxideHCID 2723790ThioureaHCID 201531881-(4-Chlorobenzyl)-4-(3-chloropropyl)homopiperazine

生成物 1

HCID 201531743-[4-(4-Chlorobenzyl)homopiperazin-1-yl]-propanethiol収率 39.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

4.1 g of thiourea were added to a mixture of 8.0 g of 1-(4-chlorobenzyl)-4-(3-chloropropyl)homopiperazine and 100 ml of reagent ethanol. The mixture was refluxed for 6 hours and then stirred overnight at room temperature. A solution of 5.0 g of sodium hydroxide in 30 ml of water was added, and the resulting solution was refluxed for 4 hours. The ethanol was removed in vacuo, and water was added to the residue. The product was extracted with methylene chloride, and the extract was dried (sodium sulfate) and concentrated to give 3.1 g (39% of theory) of 3-[4-(4-chlorobenzyl)homopiperazin-1-yl]propanethiol as a yellow oil.

後処理

  1. temperatureThe mixture was refluxed for 6 hours
  2. temperaturethe resulting solution was refluxed for 4 hours
  3. customThe ethanol was removed in vacuo, and water
  4. additionwas added to the residue
  5. extractionThe product was extracted with methylene chloride
  6. dry with materialthe extract was dried (sodium sulfate)
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-1e3196c3874c4c36b5e3a0c2fc3b6e88
出典データセット
uspto-grants-1986_10
特許番号
US04618677

関連ノート

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