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Water → HCID 20186508、化合物

HRID 2309026
ノート
印刷プレビュー

反応式

HRID 2309026 の反応式
[ClH:1].Cl.[Cl:3][C:4]1[CH:20]=[CH:19][C:7]([CH2:8][N:9]2[CH2:14][CH2:13][N:12]([CH2:15][CH2:16][CH2:17][SH:18])[CH2:11][CH2:10]2)=[CH:6][CH:5]=1.[OH-].[Na+].O.[Cl:24][CH2:25][CH2:26][N:27]1[CH2:32][CH2:31][N:30]([CH2:33][C:34]2[CH:39]=[CH:38][C:37]([Cl:40])=[CH:36][CH:35]=2)[CH2:29][CH2:28]1>C(O)C>[ClH:3].[ClH:24].[ClH:1].[ClH:3].[Cl:40][C:37]1[CH:38]=[CH:39][C:34]([CH2:33][N:30]2[CH2:31][CH2:32][N:27]([CH2:26][CH2:25][S:18][CH2:17][CH2:16][CH2:15][N:12]3[CH2:11][CH2:10][N:9]([CH2:8][C:7]4[CH:19]=[CH:20][C:4]([Cl:3])=[CH:5][CH:6]=4)[CH2:14][CH2:13]3)[CH2:28][CH2:29]2)=[CH:35][CH:36]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 12362126HCID 12362126、化合物HCID 137311183-[4-(4-Chlorobenzyl)piperazin-1-yl]propanethiol dihydrochloride

生成物 1

HCID 20186508HCID 20186508、化合物収率 96.5%

試薬・触媒・溶媒 1

HCID 702Ethanol
溶媒
2 回

実験手順

A mixture of 3-[4-(4-chlorobenzyl)piperazine-1-yl]propanethiol dihydrochloride (2 g), sodium hydroxide (0.3 g), water (10 ml), and ethanol (100 ml) is refluxed for 15 minutes, and then a solution of 1-(2-chloroethyl)-4-(4-chlorobenzyl)piperazine (1.9 g) in ethanol (20 ml) is added. The resulting mixture is refluxed for 2 hours and the ethanol is removed in vacuo. Water is added to the residue and the product is extracted with methylene chloride, dried (magnesium sulfate), and concentrated. The resulting oil is purified on a silica gel column (methylene chloride: methanol, 9:1), and then dissolved in ether. The product is precipitated with ethereal hydrochloric acid and recrystallized from aqueous ethanol to provide 1.2 g of {2-[4-(4-chlorobenzyl)piperazin-1-yl)ethyl}{3-[4-(4-chlorobenzyl)piperazin-1-yl]propyl}sulfide tetrahydrochloride as colorless crystals, m.p. 292°-295° C.

後処理

  1. temperatureis refluxed for 15 minutes
  2. temperatureThe resulting mixture is refluxed for 2 hours
  3. customthe ethanol is removed in vacuo
  4. additionWater is added to the residue
  5. extractionthe product is extracted with methylene chloride
  6. dry with materialdried (magnesium sulfate)
  7. concentrationconcentrated
  8. customThe resulting oil is purified on a silica gel column (methylene chloride: methanol, 9:1)
  9. dissolutiondissolved in ether
  10. customThe product is precipitated with ethereal hydrochloric acid
  11. customrecrystallized from aqueous ethanol

出典と根拠

ORDレコード
ord-82ae0bb0ac5549b18556205a9a7e9949
出典データセット
uspto-grants-1987_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04692448

反応ノート

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