Tulobuterol synthesis
- Product Name:Tulobuterol
- CAS Number:41570-61-0
- Molecular formula:C12H18ClNO
- Molecular Weight:227.73
2142-68-9
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$6.00/10g
75-64-9
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$10.00/10g
41570-61-0
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$65.00/10 g
Yield:41570-61-0 79%
Reaction Conditions:
Stage #1:1-(2-chlorophenyl)ethanone with N-Bromosuccinimide;toluene-4-sulfonic acid in dichloromethane for 6 h;Reflux;
Stage #2:tert-butylamine with magnesium sulfate in methanol at 30; for 4 h;Inert atmosphere;
Stage #3: with potassium borohydride in ethanol at -10 - 10; for 6.5 h;Reflux;Solvent;Reagent/catalyst;Temperature;
Steps:
1-6 Example 4
In a three-necked flask, put 100.0 g of the above compound 3 and compound 10 mixture (equivalent to 0.40 mol of compound 2), add 500 ml of methanol, add 192.0 g of anhydrous magnesium sulfate, add 116.8 g of tert-butylamine, and react at 30 ° C for 4 hours under nitrogen protection. Reduce the temperature to -10 ° C, add 12.9 g of potassium borohydride in portions, and control the temperature between -10 ° C and 10 ° C. Add potassium borohydride, react at 10 ° C for half an hour, heat up, and react at reflux for 6 hours. The reaction is completed. After treatment, 71.7 g of tulobuterol was obtained with a total molar yield of 79%.
References:
Hangzhou Bai Cheng Pharmaceutical Technology Co., Ltd.;Wu Junping;Ye Xinjie;Li Zhaoyong;Wang Chuandong;Li Yanqin CN110590569, 2019, A Location in patent:Paragraph 0015; 0031-0032; 0033-0044
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41570-61-0
124 suppliers
$65.00/10 g