2,7-Dichloro-alpha-[(dibutylamino)methyl]-9H-fluorene-4-methanol synthesis
- Product Name:2,7-Dichloro-alpha-[(dibutylamino)methyl]-9H-fluorene-4-methanol
- CAS Number:69759-61-1
- Molecular formula:C23H29Cl2NO
- Molecular Weight:406.39
53221-14-0
156 suppliers
$250.00/500 mg
111-92-2
386 suppliers
$14.00/25mL
69759-61-1
141 suppliers
$11.00/5g
Yield:69759-61-1 303 kg
Reaction Conditions:
at 140; for 6 h;Large scale;
Steps:
1
Put 235kg of intermediate into the reactor R401, add 438kg of di-n-butylamine,Warm to 140 ° C for 6 hours, take a sample, and check by TLC.When there is no corresponding point of the raw material point, the reaction ends. Cool down,Transfer to the water-added reactor R402, separate the layers, and continue to wash the organic layer twiceThe solvent di-n-butylamine in the organic layer was distilled off under reduced pressure. Steamed,Cool down to below 80 , add 1200L of absolute ethanol, stir and heat to reflux,Filter while hot, slowly lower the temperature to 0-5 , keep for 1 hour, centrifuge and spin,The filter cake was washed with about 100L of absolute ethanol to obtain intermediate wet powder,Send to the double cone dryer to dry 303kg of light yellow crystalline powder.Sample inspection, the content of intermediate V meets product quality standards.
References:
Rizhao Baluote Pharmaceutical Co., Ltd.;Liu Jialin;Huo Xiaoyong;Fang Chaojie;Zhang Yuanyuan CN111039804, 2020, A Location in patent:Paragraph 0041-0050; 0056
7012-16-0
250 suppliers
$7.00/1g
69759-61-1
141 suppliers
$11.00/5g
86-73-7
397 suppliers
$6.00/25g
69759-61-1
141 suppliers
$11.00/5g