Chloroacetyl chloride → HCID 68121302、化合物

HRID 2397578ノート

反応式

HRID 2397578 の反応式
[Cl:1][CH2:2][C:3](Cl)=[O:4].[Cl:6][C:7]1[CH:15]=[CH:14][C:13]2[N:12]3[CH2:16][CH2:17][NH:18][CH2:19][C:11]3=[C:10]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[C:9]=2[CH:8]=1.C([N:28](CC)CC)C>ClCCl>[Cl:1][CH2:2][C:3]([NH:28][CH:19]1[C:11]2=[C:10]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[C:9]3[CH:8]=[C:7]([Cl:6])[CH:15]=[CH:14][C:13]=3[N:12]2[CH2:16][CH2:17][NH:18]1)=[O:4]

参加物

5

反応物 3

HCID 6577Chloroacetyl chlorideHCID 8471TriethylamineHCID 15733250HCID 15733250、化合物

生成物 1

HCID 68121302HCID 68121302、化合物収率 54.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
39 °C

実験手順

A solution of chloracetyl chloride (4.60 g, 0.0407 mole) in dichloromethane (25 ml) is added over a period of three-fourth hours to a solution of 8chloro-10-phenyl-1,2,3,4-tetrahydropyrazino[1,2-a] indole (10.0 g, 0.0353 mole) and triethylamine (4.13 g, 0.0407 mole) in dichloromethane (100 ml). An exotherm raises the temperature to 39° C. The reaction mixture is stirred at room temperature for 6 hours, then allowed to stand overnight. It is concentrated to dryness. The residue was taken up in dichloromethane (500 ml), washed with water and saturated sodium chloride solution and dried over anhydrous sodium sulfate. The drying agent is removed by filtration and the filtrate is concentrated to dryness. The residue is recrystallized twice from isopropanol, giving the above titled product, 6.94 g (54.7% yield), melting at 139°-149° C.

後処理

  1. waitto stand overnight
  2. concentrationIt is concentrated to dryness
  3. washwashed with water and saturated sodium chloride solution
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe drying agent is removed by filtration
  6. concentrationthe filtrate is concentrated to dryness
  7. customThe residue is recrystallized twice from isopropanol

出典と根拠

ORDレコード
ord-c51b1a2454ac4dff82a03d94fe86a711
出典データセット
uspto-grants-1977_05
特許番号
US04022778

反応ノート

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