Dimethyl Sulfoxide → Quinacridone

HRID 865384ノート

反応式

HRID 865384 の反応式
CS(C)=O.[OH-:5].[K+].[OH2:7].C1(C2[C:21]3[C:20](=O)[N:19]=[C:18]([C:23]4[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=4)[C:17]=3[C:16](=O)[N:15]=2)C=CC=CC=1>CO>[CH:27]1[CH:28]=[C:23]2[C:18]([C:17]3[C:20]([NH:19][C:24]2=[CH:25][CH:26]=1)=[CH:21][C:17]1[C:18]([C:23]2[C:28]([NH:15][C:16]=1[CH:16]=3)=[CH:27][CH:26]=[CH:25][CH:24]=2)=[O:7])=[O:5]

参加物

6

反応物 4

HCID 679Dimethyl SulfoxideHCID 962WaterHCID 14797Potassium HydroxideHCID 152175761,4-Dioxo-3,6-diphenylpyrrolo[3,4-c]pyrrole

生成物 1

HCID 13976Quinacridone

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A 500 ml flask equipped with a stirrer, thermometer, and condenser is charged with 100 ml DMSO, 8.9 grams of 45% aqueous potassium hydroxide, and 9 ml water. 8.5 grams unsubstituted gamma-II-quinacridone and 1.5 grams 3,6-diphenyl-1,4-diketopyrrolo[3,4-c]pyrrole are added at 40°-50° C. The mixture is heated and stirred for 5 minutes at 80°-90° C. The resulting deep blue solution of the pigment salts is drowned into methanol at 20°-40° C., causing the pigment to precipitate. The pigment suspension is stirred at reflux temperature for 1 hour, then filtered. The presscake is washed DMSO-free with methanol, followed by water to a pH 7.0-8.0, and then dried. The pulverized pigment shows the x-ray diffraction pattern of a gamma-1-quinacridone without peaks of the DPP pigment and different from the x-ray diffraction diagram of the gamma-II-quinacridone starting material. Thus, a quinacridone/DPP pigment solid solution with the quinacridone as host is formed. The pigment solid solution shows an opaque highly saturated strong red color when applied in plastics or paints with excellent weatherfastness properties.

後処理

  1. customA 500 ml flask equipped with a stirrer
  2. temperatureThe mixture is heated
  3. customto precipitate
  4. stirringThe pigment suspension is stirred
  5. temperatureat reflux temperature for 1 hour
  6. filtrationfiltered
  7. washThe presscake is washed DMSO-free with methanol
  8. customdried

出典と根拠

ORDレコード
ord-3953aef7fc574b78bb066df15f3dbd10
出典データセット
uspto-grants-1996_10
特許番号
US05565578

反応ノート

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