ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Water → 1-Carbomethoxy-4-[4,4-bis(p-fluorophenyl)butyl]-piperazine hydrochloride

HRID 542182
ノート
印刷プレビュー

反応式

HRID 542182 の反応式
[C:1]([N:5]1[CH2:10][CH2:9][NH:8][CH2:7][CH2:6]1)([O:3][CH3:4])=[O:2].[Cl:11][CH2:12][CH2:13][CH2:14][CH:15]([C:23]1[CH:28]=[CH:27][C:26]([F:29])=[CH:25][CH:24]=1)[C:16]1[CH:21]=[CH:20][C:19]([F:22])=[CH:18][CH:17]=1.C(=O)(O)[O-].[Na+].O>C(O)C>[ClH:11].[C:1]([N:5]1[CH2:10][CH2:9][N:8]([CH2:12][CH2:13][CH2:14][CH:15]([C:16]2[CH:17]=[CH:18][C:19]([F:22])=[CH:20][CH:21]=2)[C:23]2[CH:28]=[CH:27][C:26]([F:29])=[CH:25][CH:24]=2)[CH2:7][CH2:6]1)([O:3][CH3:4])=[O:2]
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 768201,1'-(4-Chlorobutylidene)bis(4-fluorobenzene)HCID 142729Methyl piperazine-1-carboxylateHCID 516892Sodium Bicarbonate

生成物 1

HCID 202094811-Carbomethoxy-4-[4,4-bis(p-fluorophenyl)butyl]-piperazine hydrochloride収率 17.3%

試薬・触媒・溶媒 1

HCID 702
Ethanol
溶媒

実験手順

To a solution of 4.3 g (0.03 mole) 1-carbomethoxypiperazine in 10 ml of ethanol was added 10.0 g (0.036 mole) of 4-chloro-1,1-bis-(p-fluorophenyl)-butane and 5.0 g of sodium bicarbonate. The mixture was heated at reflux for 36 hours. 100 ml of water was added. The mixture was extracted twice with Et2O. The combined extracts were dried over sodium sulphate and concentrated. The residue was dissolved in ethanol-ether and the hydrochloride was precipitated with ethanolic HCl. The solid was collected by filtration and recrystallised from propan-2-ol to give 2.2 g of 1-carbomethoxy-4-[4,4-bis(p-fluorophenyl)butyl]-piperazine hydrochloride. Melting point 192°-193° C.

後処理

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 36 hours
  3. extractionThe mixture was extracted twice with Et2O
  4. dry with materialThe combined extracts were dried over sodium sulphate
  5. concentrationconcentrated
  6. dissolutionThe residue was dissolved in ethanol-ether
  7. customthe hydrochloride was precipitated with ethanolic HCl
  8. filtrationThe solid was collected by filtration
  9. customrecrystallised from propan-2-ol

出典と根拠

ORDレコード
ord-7c0001171b8048a3ad3c61c16d4fe6cc
出典データセット
uspto-grants-1987_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04656175

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート