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CIS-N-BENZYL-3-METHYLAMINO-4-METHYL-PIPERIDINE BIS-(HYDROCHLORIDE)
- Name CIS-N-BENZYL-3-METHYLAMINO-4-METHYL-PIPERIDINE BIS-(HYDROCHLORIDE)
- CAS 1062580-52-2
- Purity 99%
Product Details
Excellent chemical plant bulk supply CIS-N-BENZYL-3-METHYLAMINO-4-METHYL-PIPERIDINE BIS-(HYDROCHLORIDE) 1062580-52-2
- Molecular Formula: C14H24Cl2N2
- Molecular Weight: 291.264
- Melting Point: 249～251℃
- PSA： 15.27000
- LogP: 4.04920
CIS-N-BENZYL-3-METHYLAMINO-4-METHYL-PIPERIDINE BIS-(HYDROCHLORIDE)(Cas 1062580-52-2) Usage
|
Synthesis |
The TiCl4(0.2g, 1mmol), NEt3(0.15g, 1 . 5mmol) suspended 200 ml in toluene, then add 1-benzyl-4-methyl-3-ketone piperidine (20.3g, 100mmol), temperature control 35 °C methylamine solution is added to the reaction solution (9.32g, 120mmol) reaction 4 hours, adding NaBH (OAC) 3 (0.32g, 1 . 5mmol), glacial acetic acid 2 ml, temperature control 35 °C reaction, thin layer monitoring after the reaction is complete. Adding saturated salt water washing, anhydrous sodium sulfate for drying the organic phase, the organic phase concentrated, with residues 35% hydrochloric acid ethanol re-crystallization, to obtain (3R, 4R)-cis-1-benzyl-4-methyl-3-methylamino-piperidine dihydrochloride 17.2g, yield 85.0%, optical purity 99.0% (HPLC method). |
InChI:InChI:1S/C14H22N2.2ClH/c1-12-8-9-16(11-14(12)15-2)10-13-6-4-3-5-7-13;;/h3-7,12,14-15H,8-11H2,1-2H3;2*1H
1062580-52-2 Relevant articles
Asymmetric Synthesis of a Key Intermediate for Tofacitinib via a Dynamic Kinetic Resolution-Reductive Amination Protocol
Verzijl, Gerard K. M.,Schuster, Christian,Dax, Thomas,De Vries, André H. M.,Lefort, Laurent
, p. 1817 - 1822 (2018)
We report the first example of a catalyt...
Preparation methods of tofacitinib citrate intermediate and tofacitinib citrate
-
, (2020/01/25)
The invention discloses preparation meth...
PROCESS FOR THE PREPARATION OF CHIRAL 3-AMINO-PIPERIDINS, USEFUL INTERMEDIATES FOR THE PREPARATION OF TOFACITINIB
-
Paragraph 0112; 0113, (2019/01/15)
Object of the present invention is an im...
PROCESS FOR PREPARING CHIRAL AMINES
-
Page/Page column 16; 17, (2018/04/17)
The invention pertains to a process for ...
Preparation method for chiral piperylhydrazine compound and recycling method for chiral resolving agent
-
Paragraph 0012; 0015; 0017; 0020; 0022; 0025, (2019/01/08)
The invention discloses a preparation me...
1062580-52-2 Process route
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477600-70-7,1354621-59-2,1431697-80-1,477600-69-4
N-(3R,4R)-(1-benzyl-4-methylpiperidin-3-yl)-methylamine
-
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1062580-52-2,1228879-37-5,1354486-07-9,477600-68-3
N-((3R,4R)-1-benzyl-4-methylpiperidin-3-yl)-N-methylamine dihydrochloride
| Conditions | Yield |
|---|---|
|
With
hydrogenchloride;
In
ethanol;
at 0 - 5 ℃;
pH=3 - 4;
|
94%
|
|
With
hydrogenchloride;
In
n-heptane; isopropyl alcohol;
at 20 ℃;
for 0.666667h;
Reflux;
|
60%
|
-
-
32018-96-5
1-benzyl-4-methyl-piperidin-3-one
-
-
6998-30-7
methylamine acetate
-
-
1062580-52-2,1228879-37-5,1354486-07-9,477600-68-3
N-((3R,4R)-1-benzyl-4-methylpiperidin-3-yl)-N-methylamine dihydrochloride
-
-
1228879-37-5,1354486-07-9,477600-68-3
(3R,4R)-1-benzyl-N,4-dimethylpiperidine-3-amine dihydrochloride
| Conditions | Yield |
|---|---|
|
1-benzyl-4-methyl-piperidin-3-one; methylamine acetate;
With
bis(1,5-cyclooctadiene)diiridium(I) dichloride; (S)-3,5-di-tert-butyl-4-methoxyphenyl-(6,6’-dimethoxybiphenyl-2,2’-diyl)-bis(diphenylphosphine); hydrogen;
In
dichloromethane; isopropyl alcohol;
at 70 ℃;
for 18h;
under 37503.8 Torr;
With
hydrogenchloride;
In
dichloromethane; water; isopropyl alcohol;
Overall yield = 86%; Overall yield = 498 mg; enantioselective reaction;
|
74%
|
1062580-52-2 Upstream products
-
32018-96-5
1-benzyl-4-methyl-piperidin-3-one
-
74-89-5
methylamine
-
6998-30-7
methylamine acetate
-
384338-23-2
(1-benzyl-4-methyl-piperidin-3-yl)-methyl-amine
1062580-52-2 Downstream products
-
540737-29-9
Tofacitinib citrate
-
1260590-51-9
((3R,4R)-4-methylpiperidin-3-yl)-N-methyl-(7H-pyrrolo[2,3-d]pyrimidin-4-yl)amine dihydrochloride
-
1259404-17-5
tasocitinib
-
923036-30-0
N-((3R,4R)-1-benzyl-4-methylpiperidin-3-yl)-N-methyl-(7-p-toluenesulfonyl)-7H-pyrrolo[2,3-d]pyrimidin-4-amine
