Acetonitrile → Phthalonitrile

HRID 240206

反応式

HRID 240206 の反応式
[NH2:1][C:2]1[C:3](S(O)(=O)=O)=[CH:4][CH:5]=[C:6](S(O)(=O)=O)[CH:7]=1.[C:16](#[N:18])[CH3:17]>O>[C:2](#[N:1])[C:7]1[C:17](=[CH:3][CH:4]=[CH:5][CH:6]=1)[C:16]#[N:18]

参加物

4

反応物 2

HCID 6342AcetonitrileHCID 609882-Amino-p-benzenedisulfonic acid

生成物 1

HCID 7042Phthalonitrile

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
40 °C

実験手順

A solution of aniline 2,5 disulphonic acid (27.5 g) in water (250 ml) was added to intermediate E (63.2 g) in acetonitrile (800 ml) and heated at 40° C. and at pH 5 to 7 overnight. The reaction solvent was removed under reduced pressure, water (50 ml) was added and then brine (60 ml) the solid which precipitated of filtered off, washed with 10% brine and dried to give product (91.1% strength, 22 g).

後処理

  1. customThe reaction solvent was removed under reduced pressure, water (50 ml)
  2. additionwas added
  3. custombrine (60 ml) the solid which precipitated
  4. filtrationof filtered off
  5. washwashed with 10% brine
  6. customdried
  7. customto give product (91.1% strength, 22 g)

出典と根拠

ORDレコード
ord-fe1ef58b8c64429ab6caf2f77af6a2c5
出典データセット
uspto-grants-2014_02
特許番号
US08647425B2

関連ノート

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