Dimethyl Sulfate → Solvent Red 111

HRID 2051376

반응식

HRID 2051376 반응식
[NH2:1][C:2]1[C:15]2[C:14](=[O:16])[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[C:7](=[O:17])[C:6]=2[CH:5]=[CH:4][CH:3]=1.[OH-].[K+].[CH3:20]OS(=O)(=O)OC>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.C(O)(=O)C.ClC1C=CC=CC=1.O>[CH3:20][NH:1][C:2]1[C:15]2[C:14](=[O:16])[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[C:7](=[O:17])[C:6]=2[CH:5]=[CH:4][CH:3]=1

참가 물질

8

반응물 3

HCID 6497Dimethyl SulfateHCID 67101-AminoanthraquinoneHCID 14797Potassium Hydroxide

생성물 1

HCID 6706Solvent Red 111수율 99.5%

시약·촉매·용매 4

HCID 176Acetic Acid촉매HCID 74236Tetrabutylammonium Bromide촉매HCID 962Water용매HCID 7964Chlorobenzene용매2회

반응 조건

온도
30 °C

실험 절차

A mixture of 1-aminoanthraquinone (purity 99.6%, 22.4 g), monochlorobenzene (224 g), tetra-n-butyl ammonium bromide (3.4 g), 96% potassium hydroxide (11.7 g) and dimethylsulfuric acid (25 g) was stirred while being maintained at 30° C. for 24 hours. After water (150 g) was added, the solution was stirred for 1 hour, being maintained at 50° C. pH of the aqueous phase was 10 or higher. Then, acetic acid (0.5 g) was added for neutralization (pH of the aqueous phase being 7) and then monochlorobenzene was recovered by heating. After being cooled down to 50° C., the solution was filtered, and a solid was washed and then dried to obtain 1-methylaminoanthraquinone (23.7 g, purity 97.6%, yield 97.6%).

후처리

  1. stirringthe solution was stirred for 1 hour
  2. temperaturebeing maintained at 50° C. pH of the aqueous phase
  3. customwas recovered
  4. temperatureby heating
  5. temperatureAfter being cooled down to 50° C.
  6. filtrationthe solution was filtered
  7. washa solid was washed
  8. customdried

출처 및 근거

ORD 기록
ord-b59bfb58a7da4815814fd5d40c8f0650
출처 데이터셋
uspto-grants-1991_05
특허 번호
US05017713

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