Fluorescent Brightener 135 synthesis
- Product Name:Fluorescent Brightener 135
- CAS Number:1041-00-5
- Molecular formula:C18H14N2O2
- Molecular Weight:290.32
Yield:1041-00-5 65%
Reaction Conditions:
boric acid;toluene-4-sulfonic acid in tetralin at 220;Microwave irradiation;Cooling;
Steps:
3
Example 3; Preparation of 1,2-bis(5-methylbenzoxazol-2'-yl)ethylene; 2.3 g of fumaric acid and 5.52 g of o-amino-p-cresol were homogenized in 12.45 g of tetralin with heating and stirring. The ammonium salt-containing suspension thus prepared was admixed with 42 mg of boric acid and 12 mg of p-toluene-sulfonic acid and, with full external cooling, exposed to microwave irradiation of 300 W in the open apparatus with stirring for 30 minutes. A temperature of approx. 220° C. measured by means of an IR sensor was attained. Subsequently, the reaction mixture was cooled to room temperature within 10 minutes. The yield of 1,2-bis(5-methylbenzoxazol-2'-yl)ethylene based on fumaric acid was 65%.After filtering, washing the crystals with methanol, extracting residual acid by stirring with alcoholic sodium hydroxide solution and drying, 1,2-bis(5-methylbenzoxazol-2'-yl)ethylene was obtained with more than 98% purity.
References:
Clariant Finance Wickhams Cay US2010/76040, 2010, A1 Location in patent:Page/Page column 6
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