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Chemical Structure| 41445-40-3 Chemical Structure| 41445-40-3

Structure of 41445-40-3

Chemical Structure| 41445-40-3

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Product Details of [ 41445-40-3 ]

CAS No. :41445-40-3
Formula : C24H30N3O3P
M.W : 439.49
SMILES Code : O(C1=CC=C(C=C1)N(C)C)P(OC2=CC=C(C=C2)N(C)C)OC3=CC=C(C=C3)N(C)C
MDL No. :MFCD35058045

Safety of [ 41445-40-3 ]

GHS Pictogram:
Signal Word:Danger
Hazard Statements:H318-H410
Precautionary Statements:P273-P280-P305+P351+P338-P501
Class:9
UN#:3077
Packing Group:

Application In Synthesis of [ 41445-40-3 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

  • Downstream synthetic route of [ 41445-40-3 ]

[ 41445-40-3 ] Synthesis Path-Downstream   1~1

  • 1
  • [ 619-60-3 ]
  • [ 41445-40-3 ]
YieldReaction ConditionsOperation in experiment
With triethylamine; phosphorus trichloride; In toluene; at 0 - 20℃; for 0.5h; Example 4: Synthesis of tris(4-(dimethylamino)phenyl) phosphite (TDAPP), a palladium-binding ligand Step 2: Preparation of tris(4-(dimethylamino)phenyl) phosphite (TDAPP) Et3N (39.03 mL, 280 mmol, 1.40 equiv) was charged to the reaction mixture obtained in step 1. The batch temperature was adjusted to 2 °C (0 to 5 °C). A solution of PC13 (7.00 mL, 80 mmol, 0.40 equiv) in toluene (43.2 mL, 2 vol) was slowly charged to the reactor while maintaining the reaction temperature < 12 °C. The reaction is exothermic and the mixture becomes thick. Vigorous stirring was required for efficient mixing. The batch was agitated for 30 minutes at 15 °C (10 to 20 °C). An aliquot of the reaction was withdrawn for HPLC analysis. The reaction is deemed complete when the amount of DAP is < 2percent with respect to TDAPP. TBME (174.4 mL, 8 vol) was charged and the batch was agitated for 2 hours at 23 °C (20 to 25 °C) to ensure thorough precipitation of the Et3N HCl from the solution. The batch was filtered through a pad of celite (21.8 g, 1 wt. equiv)/silica gel (10.8 g, 0.5 wt. equiv). The pad of celite/silica gel was washed with TBME (43.2 mL, 2 vol). Precipitation of white crystals (Et3N*HCl salt) may form in the filtrate. If precipitation occurs, the filtrate should be filtered through a pad of celite/silica gel. The batch was concentrated under reduced pressure to 3 volumes (65.4 mL) at 43 °C (40 to 45 °C). 2-Methyl-2-butanol (174.4 mL, 8 vol) was charged to the batch. A precipitate may form during addition of the alcohol. The batch was then concentrated under reduced pressure to 6 vol (130.8 mL). Next, 2-methyl-2-butanol (43.2 mL, 2 vol) was charged to the batch. A thick slurry is formed after 2-methyl-2-butanol addition. An aliquot of the batch was removed to determine residual toluene content by GC-FID. The toluene content may affect the following crystallization. The batch temperature was adjusted to 63 °C (60 to 65 °C), resulting in a clear solution. The batch temperature was then adjusted to 40 - 45 °C and seeded with TDAPP seed crystals (200 mg). Following, the batch was cooled to 20-25 °C and agitated for 2 hours. The batch was filtered and the wet cake was washed with cold 2-methyl-2-butanol (43.2 mL, 2 vol). The batch was dried under reduced pressure to obtain TDAPP as a white solid. A sample was removed to monitor the drying by GC. The batch is deemed dry when the amount of 2-methyl-2-butanol is < 5,000 ppm.
 

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