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[ CAS No. 40137-22-2 ]

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Chemical Structure| 40137-22-2
Chemical Structure| 40137-22-2
Structure of 40137-22-2 * Storage: {[proInfo.prStorage]}

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Product Details of [ 40137-22-2 ]

CAS No. :40137-22-2 MDL No. :MFCD00082732
Formula : C4H11NO2 Boiling Point : 245.8°C at 760 mmHg
Linear Structure Formula :- InChI Key :N/A
M.W :105.14 g/mol Pubchem ID :2734122
Synonyms :

Safety of [ 40137-22-2 ]

Signal Word:Danger Class:8
Precautionary Statements:P501-P280-P303+P361+P353-P301+P330+P331-P304+P340+P310-P305+P351+P338+P310 UN#:2735
Hazard Statements:H314 Packing Group:
GHS Pictogram:

Application In Synthesis of [ 40137-22-2 ]

  • Upstream synthesis route of [ 40137-22-2 ]
  • Downstream synthetic route of [ 40137-22-2 ]

[ 40137-22-2 ] Synthesis Path-Upstream   1~6

  • 1
  • [ 556-52-5 ]
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YieldReaction ConditionsOperation in experiment
98.99% at 55℃; for 0.666667 h; Autoclave; Green chemistry second, synthesis of 3-methylamino-1, 2-propanediol (1) pressure test the reactor pressure test, all the test indicators all qualified before use. (2) Feeding open the hydraulic vacuum pump, the vacuum autoclave vacuum, when the inside kettle vacuum reaches up to 0.03MPa, the glycidol and liquid mono-methylamine are added to the high pressure reactor at a molar ratio of 1:10. (3) amination reaction The kettle temperature rose at 50 ° C ± 5 ° C, the pressure control at 4.1-4 · 2Mpa, and carry on reaction for 40 minutes. (4) Recovery of mono-methylamine in the vacuum under 0.080MPa conditions open mono-methylamine recovery device, recover mono-methylamine to the tank for reuse.(5) Distillation1) before distillation fractionThe autoclave was cooled less 30 ° C with a vacuum inside the autoclave was pumped into the reaction waste still, first open the water jet vacuum pump, into a jacketed steam into the distillation pot, inside the autoclave was heated, the autoclave to control the degree of vacuum from 0.06 to 0.07 MPa, reduce was observed when the condensate reg first and then the drop of outflow, the vacuum apparatus is switched to a high vacuum Roots - water ring units, carefully observe the change in the value of the digital vacuum gauge vacuum, adjusting the receiving tank a vacuum degree of 0.0990 ~ 0.0998MPa, 98.0 deg.] C before the gas-phase temperature of the condensate fraction prior to distillation in the next batch of crude product.2) the distillation of the desired productWhen the vapor temperature exceeds 98.1 deg.] C, handover, switching to the finished condensate tank to maintain the degree of vacuum of 0.0990 ~ 0.0998Mpa, vapor temperature of condensate 98.1-101.0 as the desired product, ie, 3-amino- 1, propanediol3-Methyl-1,2-propanediol yield 98.99percent, purity 99.96percent, impurity content was 0.04percent, a moisture content of 0.35percent is a colorless transparent viscous liquid.
Reference: [1] Patent: CN104844463, 2016, B, . Location in patent: Paragraph 0186-0200
[2] Patent: EP1201644, 2002, A2, . Location in patent: Page 17-20
[3] Chemische Berichte, 1899, vol. 32, p. 752
  • 2
  • [ 96-24-2 ]
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YieldReaction ConditionsOperation in experiment
82.4% With sodium hydroxide In water at 17 - 42℃; for 0.270167 h; Example 2 - Synthesis of MAPDThe microreactor described above was used for the synthesis. The reagents were injected at flow rates of: 1-CPD (cone. 99percent in water, 5.0 ml/min), NaOH (cone. 10percent, 19.4 ml/min) and methylamine (cone. 40percent, 79.1 ml/min).This gave a residence time of 1.72 minutes for the glycidol formation in the first and second chambers, and 14.5 minutes for the aminolysis in the fourth to tenth chambers, giving a total residence time of 16.21 minutes. The temperature was held at about 42 °C in the first and second chambers, and about 17 °C in the fourth to tenth chambers. In the Teflon tubing collection part the temperature was about 22 °C (ambient temperature). Samples were collected after 35 minutes from the starting point. The yield was 82.4 areapercent MAPD based on the amount of 1-CPD used.
Reference: [1] Patent: WO2012/108777, 2012, A1, . Location in patent: Page/Page column 8
[2] Patent: US2012/277471, 2012, A1, . Location in patent: Page/Page column 3-4
  • 3
  • [ 60278-98-0 ]
  • [ 40137-22-2 ]
Reference: [1] Journal of Medicinal Chemistry, 1984, vol. 27, # 8, p. 1007 - 1016
[2] Journal of Medicinal Chemistry, 1997, vol. 40, # 24, p. 3915 - 3925
  • 4
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YieldReaction ConditionsOperation in experiment
76% With methylamine In water A.
N-Methyl-1-amino-2,3-propandiol (45A)
Methylamine (172ml of a 40percent solution in water, 2 mol) was cooled to 0 °C and 2,3-epoxy-1-propanol (25g, 0.34mol) was added at a rate to maintain the temperature at or below 10 °C.
The mixture was stirred for 3 hours at 0 °C.
Excess methylamine and water was evaporated in vacuo and the product was purified by distillation at 103-105 °C, at 0.5 mm Hg, to give 25.6g (76percent) of the title compound.
Reference: [1] Patent: US5874624, 1999, A,
[2] Patent: EP804456, 2002, B1,
  • 5
  • [ 193483-80-6 ]
  • [ 40137-22-2 ]
Reference: [1] Gazzetta Chimica Italiana, 1997, vol. 127, # 3, p. 135 - 142
  • 6
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  • [ 40137-22-2 ]
  • [ 77697-86-0 ]
Reference: [1] Chemische Berichte, 1899, vol. 32, p. 756
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