반응식
OC1C2C(=O)C3C(=C([N+]([O-])=O)C=CC=3O)C(=O)C=2C([N+]([O-])=O)=CC=1.N[C:26]1[CH:31]=[CH:30][C:29]([CH2:32][CH2:33][OH:34])=[CH:28][CH:27]=1.NC1C=CC(C(CO)CO)=CC=1.NC1C=CC(C)=CC=1.COCCOCCO>>[CH:26]1[CH:27]=[CH:28][C:29]([CH2:32][CH2:33][OH:34])=[CH:30][CH:31]=1참가 물질
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- 온도
- 130 °C
실험 절차
A mixture of 19.4 g of 1,8-dihydroxy-4,5-dinitroanthraquinone, 25.0 g of a mixture consisting of about 72 % of 2-(4-aminophenyl)-ethanol, about 22 % of 2-(4-aminophenyl)propane-1,3-diol, about 3 % of 4-toluidine and by-products, and 140 g of diethylene glycol monomethyl ether is heated to 130° C. over a period of 2.5 hours. Stirring at 130-135° C. is continued for 6 hours, during which the water of the reaction is separated off by distillation. The reaction mixture is cooled to 100° C. and stirred into a mixture of 250 g of water, 250 g of ice and 110 g of 32 % hydrochloric acid. This crude dye suspension is filtered at about 20° C., and the product is washed with about 3 liters of water. After drying, 27 g of a dye mixture containing 65 % of the dye of the formula ##STR12## 13 % of the dye of the formula ##STR13## 3 % of the dye of the formula ##STR14## 7% of 1,8-dihydroxy-4-nitro-5-aminoanthraquinone, and 2-phenylpropane-1,3-diol and phenylethanol is obtained.
후처리
- customthe water of the reaction is separated off by distillation
- temperatureThe reaction mixture is cooled to 100° C.
- stirringstirred into a mixture of 250 g of water, 250 g of ice and 110 g of 32 % hydrochloric acid
- filtrationThis crude dye suspension is filtered at about 20° C.
- washthe product is washed with about 3 liters of water
- customAfter drying
- addition27 g of a dye mixture containing 65 % of the dye of the formula ##STR12## 13 % of the dye of the formula ##STR13## 3 % of the dye of the formula ##STR14## 7% of 1,8-dihydroxy-4-nitro-5-aminoanthraquinone, and 2-phenylpropane-1,3-diol
출처 및 근거
- ORD 기록
- ord-8ba5088737a041269298dfc4a45f7de2
- 출처 데이터셋
- uspto-grants-1990_10
- 특허 번호
- US04964876
연결된 노트
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