ChemicalBook CAS DataBase List 9951-A3

9951-A3 synthesis

13synthesis methods

Product Name:9951-A3
CAS Number:743461-63-4
Molecular formula:C29H30ClN3O5
Molecular Weight:536.02

Carbamic acid, N-[1,1'-biphenyl]-2-yl-, 1-[3-[[2-chloro-4-(hydroxymethyl)-5-methoxyphenyl]amino]-3-oxopropyl]-4-piperidinyl ester

743461-62-3
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743461-63-4
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Yield:743461-63-4 98%

Reaction Conditions:

Stage #1: biphenyl-2-ylcarbamic Acid 1-[2-(2-Chloro-4-hydroxymethyl-5-methoxy-phenylcarbamoyl)ethyl]piperidin-4-yl Esterwith N-ethyl-N,N-diisopropylamine in dichloromethane at -20; for 0.166667 h;
Stage #2: with sulfur trioxide pyridine complex in dichloromethane; for 6 h;

Steps:

4

Step 3) the resulting 59 g type (4) compound, with 70 g DIPEA and 86 g of dimethyl sulfoxide is dissolved in 300 ml dichloromethane in, for -20 °C stirring for 10 min, after addition of 88 g of sulfur trioxide pyridine, continue to be admitted to the completion of the reaction 6 h, to be after the reaction is complete by adding 200 ml water quenching reaction, after dichloromethane extraction, drying, desolvation to get the yellow solid, crude yield up to 98%

References:

CN106632257,2019,B Location in patent:Paragraph 0072-0077

1251456-87-7 Synthesis