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ChemicalBook CAS DataBase List Solvent Red 52

Solvent Red 52 synthesis

6synthesis methods
(a) 6-Bromo-3-methyl-3H-naphtho[1,2,3-de]quinoline-2,7-dione or 1-Bromo-4-(N-methylacetamido)anthraquinone and p-Methylaniline condensation; (b)N-(4-(p-toluidino)-9,10-dioxo-9,10-dihydroanthracen-1-yl)-N-methylacetamide closed loop into Anthrapyridone.
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Yield: 97.5%

Reaction Conditions:

with boric acid at 100 - 120;Large scale;Green chemistry;

Steps:

1-7; 9
(d) Add intermediate B to a 5000L enamel reactor, add 1200 kg of p-toluidine, 120 kg of boric acid, and raise the temperature to 100-120 ° C for condensation reaction (HPLC detection to determine the end point), then cool down to add methanol solvent to isolate, cool down Filtration to 30~40 °C, filter cake washed with 400 kg of methanol, collecting filtrate and bubble washing liquid, distilling and recovering solvent (containing p-toluidine, methanol); filter cake and then washing with 80~90 °C hot water to neutral, After drying, pulverizing and packaging, the finished product of hydrazine and pyridone dyes was 1296 kg (yield was 97.5%, ΔE 0.203, ΔC 0.019 was similar, pressure value was 0.15).

References:

Anhui Qing Keruijie New Materials Co., Ltd.;Zhou Lixia;Yang Qingshui;Tao Yimin;Liu Yong CN109705608, 2019, A Location in patent:Paragraph 0021-0027; 0029

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