ChemicalBook CAS DataBase List 10-methoxy-1,6-dimethylergoline-8beta-methanol

10-methoxy-1,6-dimethylergoline-8beta-methanol synthesis

4synthesis methods

Product Name:10-methoxy-1,6-dimethylergoline-8beta-methanol
CAS Number:35155-28-3
Molecular formula:C18H24N2O2
Molecular Weight:300.4

1774-47-6 Synthesis

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10-methoxy-6-methylergoline-8beta-methanol

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10-methoxy-1,6-dimethylergoline-8beta-methanol

35155-28-3
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Yield: 68.9%

Reaction Conditions:

with potassium hydroxide in dimethyl sulfoxide at 10 - 40; for 1.5 h;

Steps:

2 Intermediate product 2 preparation steps:
Powdered potassium hydroxide 65gAdded dimethyl sulfoxide 400g,Stir for 10 minutes,Add 10α-methoxy-dihydroergoline (Intermediate 1),Control temperature is 10-40 °C,Stir the reaction for 30 minutes,Add trimethylsulfoxonium iodide andDimethyl sulfoxide mixed solution,Trimethylsulfoxonium iodide is 120g.Dimethyl sulfoxide 480ml,After the addition was complete, the reaction was continued for 1 hour. TLC detected the progress of the reaction (UV.254, methanol, chloroform, and ammonia in a volume ratio of 1:8:0.1) After the reaction is completed, the reaction solution is poured into 2000 g of ice water and extracted three times with chloroform (1000 ml*3).After washing with purified water, the solvent was distilled off under reduced pressure, and the residue was recrystallized from 500 ml of acetone to obtain 1-methyl-10α-methoxy-dihydroergoline.(Intermediate product 2) 58.8 g, yield 68.9%.

References:

Guangzhou Puxing Pharmaceutical Co., Ltd.;He Yanan;Chen Xiuxiu;Deng Tuanfei CN107936010, 2018, A Location in patent:Paragraph 0050; 0055

35121-60-9
31 suppliers
$496.67/5MG