Lawesson's reagent → 7-nitro-1(2H)-phthalazinethione

HRID 1090711

反応式

HRID 1090711 の反応式
[N+:1]([C:4]1[CH:13]=[C:12]2[C:7]([CH:8]=[N:9][NH:10][C:11]2=O)=[CH:6][CH:5]=1)([O-:3])=[O:2].COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:24])=CC=1>C(#N)C>[N+:1]([C:4]1[CH:13]=[C:12]2[C:7]([CH:8]=[N:9][NH:10][C:11]2=[S:24])=[CH:6][CH:5]=1)([O-:3])=[O:2]

参加物

4

反応物 2

HCID 87949Lawesson's reagentHCID 2777297-Nitrophthalazin-1(2h)-one

生成物 1

HCID 199137107-nitro-1(2H)-phthalazinethione

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

13.9 g of 7-nitro-1(2H)-phthalazinone and 16.3 g of Lawesson reagent in 170 ml of acetonitrile are heated under reflux for 45 minutes. The reaction mixture is filtered while hot. The filtrate is cooled in an ice-bath and the crystals obtained are removed by filtration under suction. After drying in vacuo and recrystallization there is obtained 7-nitro-1(2H)-phthalazinethione as yellow crystals of m.p. 233°-234° (methanol/acetonitrile).

後処理

  1. temperatureunder reflux for 45 minutes
  2. filtrationThe reaction mixture is filtered while hot
  3. temperatureThe filtrate is cooled in an ice-bath
  4. customthe crystals obtained
  5. customare removed by filtration under suction
  6. customAfter drying in vacuo
  7. customrecrystallization there

出典と根拠

ORDレコード
ord-c5c7abe7f99e44569aa006873ce3179c
出典データセット
uspto-grants-1992_01
特許番号
US05082842

関連ノート

読み込み中…