Triethylamine → 1-Methyl-3-phenyl-4-(4-chlorophenacyl) piperazine

HRID 622779

反応式

HRID 622779 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][NH:5][CH:4]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH2:3]1.C(N(CC)CC)C.[Cl:21][C:22]1[CH:31]=[CH:30][C:25]([C:26](=[O:29])[CH2:27]Br)=[CH:24][CH:23]=1.C(=O)(O)[O-].[Na+]>O1CCCC1.C(Cl)(Cl)Cl>[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([CH2:27][C:26]([C:25]2[CH:30]=[CH:31][C:22]([Cl:21])=[CH:23][CH:24]=2)=[O:29])[CH:4]([C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=2)[CH2:3]1

参加物

7

反応物 4

HCID 8471TriethylamineHCID 68303p-Chlorophenacyl bromideHCID 516892Sodium BicarbonateHCID 27600091-Methyl-3-phenylpiperazine

生成物 1

HCID 143023441-Methyl-3-phenyl-4-(4-chlorophenacyl) piperazine収率 95%

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a stirred mixture of 14.0 g (0.08 mol) of 1-methyl-3-phenylpiperazine and 20 g (0.2 mol) of triethylamine in 160 ml of tetrahydrofuran was added dropwise a solution of 18.2 g (0.08 mol) of 4-chlorophenacyl bromide in 55 ml of chloroform. The resulting mixture was stirred at ambient temperature for 3.5 hours, poured into 50% aqueous sodium bicarbonate and extracted with chloroform. The organic extracts were combined, washed with water and saturated sodium chloride and dried over sodium sulfate. The filtrate was concentrated to dryness to give 25 g of crude 1-methyl-3-phenyl-4-(4-chlorophenacyl) piperazine. This material was used as such in the next step of the process.

後処理

  1. extractionextracted with chloroform
  2. washwashed with water and saturated sodium chloride
  3. dry with materialdried over sodium sulfate
  4. concentrationThe filtrate was concentrated to dryness

出典と根拠

ORDレコード
ord-8f0182d5fffe48fb93eae2b4751f2601
出典データセット
uspto-grants-1988_09
特許番号
US04772705

関連ノート

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