Methylamine → N-methyl-6-nitro-1,3-dioxaindan-5-amine

HRID 579688

반응식

HRID 579688 반응식
[CH2:1]1[O:9][C:8]2[C:3](=[CH:4][C:5]([N+:13]([O-])=O)=[C:6]([N+:10]([O-:12])=[O:11])[CH:7]=2)[O:2]1.[CH3:16]N>C(O)C>[CH3:16][NH:13][C:5]1[CH:4]=[C:3]2[O:2][CH2:1][O:9][C:8]2=[CH:7][C:6]=1[N+:10]([O-:12])=[O:11]

참가 물질

4

반응물 2

HCID 6329MethylamineHCID 6113255,6-Dinitro-1,3-benzodioxole

생성물 1

HCID 13742671N-methyl-6-nitro-1,3-dioxaindan-5-amine

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

0.05 mol (10.6 g) of 4,5-methylenedioxy-1,2-dinitrobenzene is added to 40 ml of a 33% strength solution of methylamine in absolute ethanol to which 20 ml of 96° strength ethanol have been added. The reaction edium is heated under reflux for 30 minutes. After dilution with 150 ml of ice-cold water, the expected product precipitates. After being drained and washed with water, it is recrystallized from a mixture of ethanol and acetone. It melts at 170° C. (literature 171° C.).

후처리

  1. additionhave been added
  2. temperatureThe reaction edium is heated
  3. temperatureunder reflux for 30 minutes
  4. customAfter dilution with 150 ml of ice-cold water, the expected product precipitates
  5. washwashed with water, it
  6. customis recrystallized from a mixture of ethanol and acetone
  7. customIt melts at 170° C. (literature 171° C.)

출처 및 근거

ORD 기록
ord-0e8e693e1afa4941b8829c7dfb596853
출처 데이터셋
uspto-grants-1988_06
특허 번호
US04749379

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