4-Sulfophthalic acid → Phthaloperinone sulphochloride

HRID 2398070

反応式

HRID 2398070 の反応式
[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]

参加物

7

反応物 4

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

生成物 1

HCID 86734752Phthaloperinone sulphochloride収率 91.4%

試薬・触媒・溶媒 2

HCID 7237O-Xylene溶媒HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-81a6fe1d67a5465a8a61445368ca5662
出典データセット
uspto-grants-1977_05
特許番号
US04024144

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