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

HRID 127449

反応式

HRID 127449 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 recystallized 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 structure 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.)

出典と根拠

ORDレコード
ord-15a0016f5e2a4643903fc71c61d06e76
出典データセット
uspto-grants-1981_03
特許番号
US04255580

関連ノート

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