3,6-Dimethoxybenzene-1,2-diamine → HCID 136161824、化合物

HRID 2418473ノート

反応式

HRID 2418473 の反応式
[CH3:1][O:2][C:3]1[C:4]([NH2:12])=[C:5]([NH2:11])[C:6]([O:9][CH3:10])=[CH:7][CH:8]=1.[O:13]=[C:14]1[C:23]2[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=2)[C:17](=O)[C:16](OC)=[C:15]1[C:27]([O:29][CH2:30][CH3:31])=[O:28]>C(O)C>[OH:13][C:14]1[C:15]([C:27]([O:29][CH2:30][CH3:31])=[O:28])=[C:16]2[C:17]([N:12]=[C:4]3[C:5](=[N:11]2)[C:6]([O:9][CH3:10])=[CH:7][CH:8]=[C:3]3[O:2][CH3:1])=[C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][C:23]=12

参加物

4

反応物 2

HCID 116296603,6-Dimethoxybenzene-1,2-diamineHCID 13112774HCID 13112774、化合物

生成物 1

HCID 136161824HCID 136161824、化合物収率 92.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

In 50 ml of hot ethanol was dissolved 1.68 g of 3,6-dimethoxy-o-phenylenediamine. To this solution was gradually added 2.6 g of ethyl 1,4-dihydro-1,4-dioxo-3-methoxy-2-naphthoate under heating with stirring, and the mixture was refluxed for a further 2 hours. The reaction mixture was cooled and the precipitated solid was collected by filtration and recrystallized from benzene to give 3.50 g (92.6% yield) of ethyl 5-hydroxy-8,11-dimethoxybenzo[a]-phenazine-6-carboxylate as red needles, m.p. 290° C. (decomp.), Anal. Calcd.: (%) for C21H18N2O5 ; C, 66.66; H, 4.80; N, 7.40; Found: C, 66.46; H, 4.56; N, 7.53

後処理

  1. temperatureunder heating
  2. temperaturethe mixture was refluxed for a further 2 hours
  3. temperatureThe reaction mixture was cooled
  4. filtrationthe precipitated solid was collected by filtration
  5. customrecrystallized from benzene

出典と根拠

ORDレコード
ord-fd497240f7494748842d83bbce860fcb
出典データセット
uspto-grants-1984_09
特許番号
US04472578

反応ノート

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