Hydrogen Peroxide → 5,6-bis(4-methoxyphenyl)-1,2,4-triazin-3(2h)-one

HRID 889830ノート

反応式

HRID 889830 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[C:14]([C:15]3[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[CH:17][CH:16]=3)=[N:13][NH:12][C:11](=S)[N:10]=2)=[CH:5][CH:4]=1.[OH-:24].[Na+].OO>O>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[C:14]([C:15]3[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[CH:17][CH:16]=3)=[N:13][NH:12][C:11](=[O:24])[N:10]=2)=[CH:5][CH:4]=1

参加物

5

反応物 3

HCID 784Hydrogen Peroxide2 回HCID 14798Sodium HydroxideHCID 42600365,6-bis-(4-methoxyphenyl)-1,2,4-triazin-3-thione

生成物 1

HCID 2310985,6-bis(4-methoxyphenyl)-1,2,4-triazin-3(2h)-one収率 94.2%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A slurry of 9.6 g of 5,6-bis-(4-methoxyphenyl)-1,2,4-triazin-3-thione (29.5 mmol) in 100 mL of water was treated with 2.64 g of 50% aqueous sodium hydroxide (33 mmol). Most of the solids dissolved. The reaction mixture was cooled in an ice bath and 3.8 g of 30% hydrogen peroxide (33 mmol) was added slowly. An additional 4 mL of hydrogen peroxide solution was added, and the reaction mixture was stirred overnight at room temperature. The solids were filtered, washed with water, and dried under vacuum to give 8.6 g of product, mp 238–242° C.

後処理

  1. dissolutionMost of the solids dissolved
  2. temperatureThe reaction mixture was cooled in an ice bath
  3. filtrationThe solids were filtered
  4. washwashed with water
  5. customdried under vacuum

出典と根拠

ORDレコード
ord-f46f46b796a44dfa844749a081aa6281
出典データセット
uspto-grants-2006_02
特許番号
US06995157B2

反応ノート

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