Sodium Hydroxide → 7,8-Dihydro-5-(3,4-dimethoxyphenyl)-8-methyl-7-(2,4,6-trimethylphenylimino)-1,2,4-triazolo[4,3-a]pyrimidine

HRID 4332ノート

反応式

HRID 4332 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]2[N:16]=[C:15]([NH:17][NH:18][CH:19]=O)[N:14]([CH3:21])[C:13](=[N:22][C:23]3[C:28]([CH3:29])=[CH:27][C:26]([CH3:30])=[CH:25][C:24]=3[CH3:31])[CH:12]=2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].[OH-].[Na+]>O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]2[N:16]3[CH:19]=[N:18][N:17]=[C:15]3[N:14]([CH3:21])[C:13](=[N:22][C:23]3[C:28]([CH3:29])=[CH:27][C:26]([CH3:30])=[CH:25][C:24]=3[CH3:31])[CH:12]=2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 201523173,4-Dihydro-6-(3,4-dimethoxyphenyl)-2-(2-formylhydrazino)-3-methyl-4-(2,4,6-trimethylphenylimino)pyrimidine

生成物 1

HCID 201523037,8-Dihydro-5-(3,4-dimethoxyphenyl)-8-methyl-7-(2,4,6-trimethylphenylimino)-1,2,4-triazolo[4,3-a]pyrimidine収率 83.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
110 °C

実験手順

The mixture of 3,4-dihydro-6-(3,4-dimethoxyphenyl)-2-(2-formylhydrazino)-3-methyl-4-(2,4,6-trimethylphenylimino)pyrimidine (0.81 g) and polyphosphoric acid (8.2 g, 116% as phosphoric acid) was stirred at 110° C. for 2 hours and cooled to ambient temperature. The reaction mixture was poured into water and neutralized with aqueous sodium hydroxide solution. The precipitates were collected by filtration and washed with water to give 7,8-dihydro-5-(3,4-dimethoxyphenyl)-8-methyl-7-(2,4,6-trimethylphenylimino)-1,2,4-triazolo[4,3-a]pyrimidine (0.65 g).

後処理

  1. temperaturecooled to ambient temperature
  2. filtrationThe precipitates were collected by filtration
  3. washwashed with water

出典と根拠

ORDレコード
ord-9337e50ccd674af7a4a11996c30facfa
出典データセット
uspto-grants-1988_02
特許番号
US04725600

反応ノート

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