Novel method for synthesizing cis-1-benzyl-3-methylamino-4-methyl-piperidine
A kind of methylamino, benzyl technology
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preparation Embodiment 1
[0030] Preparation Example 1: Synthesis of Compound 6 and Preparation of Intermediates
[0031] Add 4-amino-3-picoline 10 (10 g, 92.4 mmol) to a 250 ml reaction flask, add methanol (100 g), start stirring, and when the temperature is lower than 30 degrees, add sodium methoxide (7.48 g, 138.6 mmol ), add paraformaldehyde (5.54 g, 184 mmol), and complete the addition. The reaction solution was stirred overnight, and the HPLC detected that the raw material was less than 3%, and it was judged that the first-stage reaction was completed. At a temperature lower than 30°C, sodium borohydride (7.0 g, 184.8 mmol) was added in batches and stirred for 5-8 hours. The HPLC detection of raw materials was less than 3%, and the reaction was judged to be complete. The reaction solution was concentrated under reduced pressure to half, and the reaction was quenched with 3M hydrochloric acid at a temperature lower than 30 degrees, extracted twice with dichloromethane, the organic phases were com...
preparation Embodiment 2
[0034] Preparation Example 2: Synthesis of Compound 6
[0035] Add 4-amino-3-picoline 10 (10 g, 92.4 mmol) to a 250 ml reaction flask, add methanol (100 g), start stirring, and when the temperature is lower than 30 degrees, add sodium methoxide (11.22 g, 207.9 mmol ), add paraformaldehyde (2.77 g, 92 mmol), and complete the addition. The reaction solution was stirred overnight, and the HPLC detected that the raw material was less than 3%, and it was judged that the first-stage reaction was completed. At a temperature lower than 30°C, sodium borohydride (3.5g, 92.4mmol) was added in batches and stirred for 5-8 hours. The HPLC detection of raw materials was less than 3%, and the reaction was judged to be complete. The reaction solution was concentrated under reduced pressure to half, and the reaction was quenched with 3M hydrochloric acid at a temperature lower than 30 degrees, extracted twice with dichloromethane, the organic phases were combined, and concentrated under reduce...
preparation Embodiment 3
[0036] Preparation Example 3: Synthesis of Compound 6
[0037] Add 4-amino-3-picoline 10 (10 g, 92.4 mmol) to a 250 ml reaction flask, add methanol (100 g), start stirring, and when the temperature is lower than 30 degrees, add sodium methoxide (4.99 g, 92.4 mmol ), add paraformaldehyde (8.31 g, 277mmol), and complete the addition. The reaction solution was stirred overnight, and the HPLC detected that the raw material was less than 3%, and it was judged that the first-stage reaction was completed. At a temperature lower than 30°C, sodium borohydride (3.5 g, 92.4 mmol) was added in batches and stirred for 5-8 hours. HPLC detected that the raw material was less than 3%, and the reaction was judged to be complete. The reaction solution was concentrated under reduced pressure to half, and the reaction was quenched with 3M hydrochloric acid at a temperature lower than 30 degrees, extracted twice with dichloromethane, the organic phases were combined, and concentrated under reduce...
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