Water → N-(4-methyl-1-piperazinyl)-7-nitro-1,4-benzodioxane-5-carboxamide

HRID 2286975

反応式

HRID 2286975 の反応式
[NH2:1][N:2]1[CH2:7][CH2:6][N:5]([CH3:8])[CH2:4][CH2:3]1.[N+:9]([C:12]1[CH:13]=[C:14]([C:22](Cl)=[O:23])[C:15]2[O:20][CH2:19][CH2:18][O:17][C:16]=2[CH:21]=1)([O-:11])=[O:10].O>C(C(C)=O)C>[CH3:8][N:5]1[CH2:6][CH2:7][N:2]([NH:1][C:22]([C:14]2[C:15]3[O:20][CH2:19][CH2:18][O:17][C:16]=3[CH:21]=[C:12]([N+:9]([O-:11])=[O:10])[CH:13]=2)=[O:23])[CH2:3][CH2:4]1

参加物

5

反応物 3

HCID 962WaterHCID 813491-Amino-4-methylpiperazineHCID 205447457-Nitro-1,4-benzodioxane-5-carbonyl chloride

生成物 1

HCID 20544699N-(4-methyl-1-piperazinyl)-7-nitro-1,4-benzodioxane-5-carboxamide収率 55.8%

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

反応条件

温度
10 °C

実験手順

33 g of 1-amino-4-methylpiperazine were dissolved in 630 ml of methyl ethyl ketone. The mixture was cooled to 10° C. and 61 g of 7-nitro-1,4-benzodioxane-5-carbonyl chloride were introduced by portions. The mixture was stirred for two hours and then the solid was filtered off and washed with 150 ml of methyl ethyl ketone. The obtained product was purified by transformation into the base (M.P.: 212° C.) and recrystallized by treatment with hydrochloric ethanol. 45 g of N-(4-methyl-1-piperazinyl)-7-nitro-1,4-benzodioxane-5-carboxamide were obtained (M.P.: 210° C. with one mole of water). The structue was confirmed by nuclear magnetic resonance and infrared analyses.

後処理

  1. filtrationthe solid was filtered off
  2. washwashed with 150 ml of methyl ethyl ketone
  3. customThe obtained product was purified by transformation into the base (M.P.: 212° C.)
  4. customrecrystallized by treatment with hydrochloric ethanol

出典と根拠

ORDレコード
ord-854946c1cb404c2695affc55e81af2dc
出典データセット
uspto-grants-1981_05
特許番号
US04268512

関連ノート

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