3-Nitrophthalic anhydride → 1,4-Phthalazinedione, 2,3-dihydro-5-nitro-

HRID 41964

反応式

HRID 41964 の反応式
[N+:1]([C:4]1[CH:14]=[CH:13][CH:12]=[C:6]2[C:7]([O:9][C:10](=O)[C:5]=12)=[O:8])([O-:3])=[O:2].O.[NH2:16][NH2:17]>C(O)(=O)C>[N+:1]([C:4]1[CH:14]=[CH:13][CH:12]=[C:6]2[C:5]=1[C:10](=[O:9])[NH:16][NH:17][C:7]2=[O:8])([O-:3])=[O:2]

参加物

4

反応物 2

HCID 216313-Nitrophthalic anhydrideHCID 24654Hydrazine hydrate (1:1)

生成物 1

HCID 35252231,4-Phthalazinedione, 2,3-dihydro-5-nitro-収率 92%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
80 °C

実験手順

A glass flask of the volume 1 l provided with an agitator, a thermometer, a condenser and a capillary was filled with 600 ml of icy acetic acid and 154.5 g (0.8 mole) of 3-nitrophthalic acid anhydride, thereafter it was heated to the temperature of 110° C. and gradually 44.1 g (0.88 mole) of hydrazine hydrate was added. Next the reaction mixture was kept at the state of boiling for 30 minutes thereafter it was cooled to the temperature of 80° C., the crystals of 5-nitro-2,3-dihydrophthalazine-1,4-dione were filtered, the sediment was washed on a filter with 50 ml of acetic acid and two times with 40 ml of distilled water. The total amount of 5-nitro-2,3-dihydrophthalazine-1,4-dione was 228.7 g, the yield was 92%.

後処理

  1. customA glass flask of the volume 1 l provided with an agitator
  2. additionwas added
  3. filtrationthe crystals of 5-nitro-2,3-dihydrophthalazine-1,4-dione were filtered
  4. washthe sediment was washed on
  5. filtrationa filter with 50 ml of acetic acid and two times with 40 ml of distilled water

出典と根拠

ORDレコード
ord-9911b083cac04d16b4d8d7c9b4d66c81
出典データセット
uspto-grants-2013_09
特許番号
US08536171B2

関連ノート

読み込み中…