Acetonitrile → Phthalonitrile

HRID 240206

반응식

HRID 240206 반응식
[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]

참가 물질

4

반응물 2

HCID 6342AcetonitrileHCID 609882-Amino-p-benzenedisulfonic acid

생성물 1

HCID 7042Phthalonitrile

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
40 °C

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-fe1ef58b8c64429ab6caf2f77af6a2c5
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08647425B2

연결된 노트

불러오는 중…