4-Sulfophthalic acid → Phthaloperinone sulphochloride

HRID 2398070

반응식

HRID 2398070 반응식
[S:1]([C:5]1[C:6](=[O:25])[C:7]2[N:8]3[C:16]([N:17]=[C:18]4[C:24]=2[C:22]([CH:23]=1)=[CH:21][CH:20]=[CH:19]4)=[C:15]1[C:10]([CH:11]=[CH:12][CH:13]=[CH:14]1)=[CH:9]3)([OH:4])(=[O:3])=[O:2].S(C1C=C(C(O)=O)C(=CC=1)C(O)=O)(O)(=O)=O.C1C=C(N)C2C(N)=CC=CC=2C=1.P(Cl)(Cl)([Cl:56])=O>CN1CCCC1=O.C1(C)C(C)=CC=CC=1>[C:6]1(=[O:25])[C:7]2=[C:24]3[C:18](=[N:17][C:16]4[N:8]2[CH:9]=[C:10]2[C:15]=4[CH:14]=[CH:13][CH:12]=[CH:11]2)[CH:19]=[CH:20][CH:21]=[C:22]3[CH:23]=[CH:5]1.[S:1]([Cl:56])([OH:4])(=[O:3])=[O:2]

참가 물질

7

반응물 4

HCID 69624-Sulfophthalic acidHCID 24813Phosphorus oxychlorideHCID 680671,8-DiaminonaphthaleneHCID 21434658Sulphophthaloperinone

생성물 1

HCID 86734752Phthaloperinone sulphochloride수율 91.4%

시약·촉매·용매 2

HCID 7237O-Xylene용매HCID 13387N-methyl-2-pyrrolidone용매

반응 조건

온도
80 °C

실험 절차

11.5 g of sulphophthaloperinone, prepared from 4-sulphophthalic acid and 1,8-naphthylenediamine in N-methylpyrrolidone, are suspended in 100 ml of xylene. 9.2 g of phosphorus oxychloride are added and the mixture is heated to 80° C for 6 - 7 hours, whilst stirring. 25 - 30 ml of xylene are then distilled off under reduced pressure and after cooling the reaction product which has precipitated is filtered off and the residue is rinsed with petroleum ether. 11.6 g of phthaloperinone-sulphochloride are obtained.

후처리

  1. distillation25 - 30 ml of xylene are then distilled off under reduced pressure
  2. temperatureafter cooling the reaction product which
  3. customhas precipitated
  4. filtrationis filtered off
  5. washthe residue is rinsed with petroleum ether

출처 및 근거

ORD 기록
ord-81a6fe1d67a5465a8a61445368ca5662
출처 데이터셋
uspto-grants-1977_05
특허 번호
US04024144

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