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N,N-dimethyl-m-phenylenediamine → HCID 68527719, 화합물

HRID 2222242
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인쇄 미리보기

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HRID 2222242 반응식
CS([C:5]1[N:10]=[C:9]2[N:11]([CH3:26])[C:12](=[O:25])[N:13]([C:15]3[CH:20]=[C:19]([N+:21]([O-:23])=[O:22])[CH:18]=[CH:17][C:16]=3[CH3:24])[CH2:14][C:8]2=[CH:7][N:6]=1)(=O)=O.[CH3:27][N:28]([CH3:36])[C:29]1[CH:30]=[C:31]([CH:33]=[CH:34][CH:35]=1)[NH2:32]>CO>[CH3:27][N:28]([CH3:36])[C:29]1[CH:30]=[C:31]([NH:32][C:5]2[N:10]=[C:9]3[N:11]([CH3:26])[C:12](=[O:25])[N:13]([C:15]4[CH:20]=[C:19]([N+:21]([O-:23])=[O:22])[CH:18]=[CH:17][C:16]=4[CH3:24])[CH2:14][C:8]3=[CH:7][N:6]=2)[CH:33]=[CH:34][CH:35]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 76084N,N-dimethyl-m-phenylenediamineHCID 685260247-methanesulfonyl-1-methyl-3-(2-methyl-5-nitro-phenyl)-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one

생성물 1

HCID 68527719HCID 68527719, 화합물수율 58%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
130 °C

실험 절차

A mixture of 7-methanesulfonyl-1-methyl-3-(2-methyl-5-nitro-phenyl)-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one (148 mg, 0.39 mmol) and 3-dimethylaminoaniline (530 mg, 3.9 mmol) is stirred for 1 hour at 130° C. The mixture is cooled down to room temperature and suspended in methanol. The precipitate is collected and washed with methanol to give 7-(3-dimethylamino-phenylamino)-1-methyl-3-(2-methyl-5-nitro-phenyl)-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one (98 mg, 58%) as a yellow solid.

후처리

  1. temperatureThe mixture is cooled down to room temperature
  2. customThe precipitate is collected
  3. washwashed with methanol

출처 및 근거

ORD 기록
ord-d9343d5529f04aa0897cd389e7301057
출처 데이터셋
uspto-grants-2008_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07371750B2

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