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

HRID 2286975

반응식

HRID 2286975 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

반응 조건

온도
10 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-854946c1cb404c2695affc55e81af2dc
출처 데이터셋
uspto-grants-1981_05
특허 번호
US04268512

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