Acetic Acid → 2-methyl-4-(4-methylsulfonylphenyl)-1-(2H)-phthalazinone

HRID 54982ノート

反応式

HRID 54982 の反応式
[CH3:1][N:2]1[N:11]=[C:10]([C:12]2[CH:17]=[CH:16][C:15]([S:18][CH3:19])=[CH:14][CH:13]=2)[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]1=[O:20].OO.[OH2:23].C(O)(=[O:26])C>>[CH3:1][N:2]1[N:11]=[C:10]([C:12]2[CH:17]=[CH:16][C:15]([S:18]([CH3:19])(=[O:26])=[O:23])=[CH:14][CH:13]=2)[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]1=[O:20]

参加物

5

反応物 4

HCID 176Acetic AcidHCID 784Hydrogen Peroxide3 回HCID 962WaterHCID 199570882-methyl-4-(4-methylthiophenyl)-1-(2H)-phthalazinone

生成物 1

HCID 199570702-methyl-4-(4-methylsulfonylphenyl)-1-(2H)-phthalazinone収率 93%

反応条件

温度
35 °C

実験手順

To a solution of 2-methyl-4-(4-methylthiophenyl)-1-(2H)-phthalazinone (14.15 g, 0.05 mol) in acetic acid (330 mL) was added 30% H2O2 (22 mL). The mixture was heated to 35° C. overnight, additional 30% H2O2 (10 mL) was added and the mixture was stirred at 35° C. for 2 hours and finally one final portion of 30% H2O2 (10 mL) was added and the mixture was stirred for another 2 hours at 35° C. The reaction mixture was poured into water (1 L)/ice and the solid thus obtained was collected by filtration, washed with water, then ether, and then was dried to afford 14.6 g (93%) of 2-methyl-4-(4-methylsulfonylphenyl)-1-(2H)-phthalazinone as a pale yellow solid, m.p. 218°-220° C. when recrystallized from ethanol/chloroform (2×).

後処理

  1. stirringthe mixture was stirred for another 2 hours at 35° C
  2. customthe solid thus obtained
  3. filtrationwas collected by filtration
  4. washwashed with water
  5. dry with materialether, and then was dried

出典と根拠

ORDレコード
ord-b9bf489fb3764852b2277852092ff041
出典データセット
uspto-grants-1997_04
特許番号
US05624922

反応ノート

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