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

HRID 889830노트

반응식

HRID 889830 반응식
[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

참가 물질

5

반응물 3

HCID 784Hydrogen Peroxide2회HCID 14798Sodium HydroxideHCID 42600365,6-bis-(4-methoxyphenyl)-1,2,4-triazin-3-thione

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f46f46b796a44dfa844749a081aa6281
출처 데이터셋
uspto-grants-2006_02
특허 번호
US06995157B2

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