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[ CAS No. 441752-75-6 ] {[proInfo.proName]}

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Chemical Structure| 441752-75-6
Chemical Structure| 441752-75-6
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Product Details of [ 441752-75-6 ]

CAS No. :441752-75-6 MDL No. :
Formula : C10H19NO3 Boiling Point : -
Linear Structure Formula :- InChI Key :-
M.W :201.26 Pubchem ID :-
Synonyms :

Safety of [ 441752-75-6 ]

Signal Word:Warning Class:
Precautionary Statements:P261-P264-P271-P280-P302+P352-P304+P340-P305+P351+P338-P312-P362-P403+P233-P501 UN#:
Hazard Statements:H315-H319-H335 Packing Group:
GHS Pictogram:

Application In Synthesis of [ 441752-75-6 ]

* 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 [ 441752-75-6 ]

[ 441752-75-6 ] Synthesis Path-Downstream   1~3

  • 1
  • [ 26690-80-2 ]
  • [ 106-95-6 ]
  • [ 441752-75-6 ]
YieldReaction ConditionsOperation in experiment
88% With sodium hydroxide; tetra-(n-butyl)ammonium iodide In dichloromethane; water at 20℃; for 15h;
86% With tetrabutylammomium bromide; sodium hydroxide In dichloromethane at 25℃; for 12h; Inert atmosphere; 1 Step 1 - Tert-butyl N-(2-allyloxyethyl)carbamate To a mixture of tert-butyl N-(2-hydroxyethyl)carbamate (5.00 g, 31.0 mmol, 4.81 mL, CAS 26690-80-2) and TBAB (7.00 g, 21.7 mmol) in DCM (60 mL) was added 3-bromoprop- 1-ene (4.13 g, 34.1 mmol, CAS 106-95-6) and NaOH (10 M, 31 mL). The reaction mixture was stirred at 25 °C for 12 hours. On completion, the reaction mixture was diluted with water (50 mL) and extracted with DCM (2 X 100 mL). The combined organic layers was dried over Na2SO4, filtered and concentrated in vacuo to give a residue. The residue was purified by column chromatography to give the title compound (5.40 g, 86% yield) as colorless oil.1H NMR (400 MHz, CDCl3) d 5.97 - 5.82 (m, 1H), 5.32 - 5.25 (m, 1H), 5.22 - 5.17 (m, 1H), 4.91 (s, 1H), 4.03 - 3.94 (m, 2H), 3.55 - 3.42 (m, 2H), 3.38 - 3.25 (m, 2H), 1.45 (s, 9H).
With sodium hydroxide; benzyltrimethylammonium chloride In dichloromethane; water for 19h; 13.B Part B Sodium hydroxide (1.50 L of 50% aqueous) was added to a solution of 243.8 g (1.514 mole) of material from Part A in dichloromethane (3 L). Benzyltrimethylammonium chloride (28.1 g, 0.151 mole) was added. The reaction mixture was placed in a water bath (25° C.) and stirred vigorously. Allyl bromide (144 mL, 1.66 mole) was added in a single portion. The reaction mixture was stirred for a total of 19 hours at which time analysis by TLC indicated that all of the starting material had been consumed. The reaction mixture was divided into two portions and each portion was worked up in the following manner. The reaction mixture was diluted with ice water (1 L). The phases were separated. The aqueous phase was extracted with dichloromethane (3*1 L). The combined organics were washed sequentially with water (3*1 L) and brine (2*1 L), dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure. The two portions were combined to provide 269.6 g of tert-butyl [2-(allyloxy)ethyl]carbamate as a colorless oil.
With tetrabutylammomium bromide; sodium hydroxide In dichloromethane; water at 24℃; for 19h; Tert-butyl allylcarbamate (3) 10 M aq. NaOH (21 mL), TBAB (5.58 g, 17.30 mmol) and allyl bromide (2.15 mL, 24.90 mmol) were successively added to a solution of compound 2 (3.60 g, 22.50 mmol) in DCM (40 mL). The reaction mixture was stirred at 24 for 19 h, washed with cold water (15 mL). The aqueous phase was washed with DCM (4 × 25 mL). The combined organic phase was washed with brine (2 30 mL), dried over Na2SO4, filtered, and evaporated to dryness in vacuo. The crude product 3 was obtained (4.18 g) and used without further purification. 1H NMR (300 MHz): 1.37 (s, 9 H, C(CH3)3), 3.91 (d, J = 5.6, 2 H, NCH2CH=CH2), 5.06 - 5.25 (m, 2 H, NCH2CH=CH2), 5.71 - 5.89 (m, 1 H, NCH2CH=CH2). 13 NMR (75 MHz): 28.37, 40.41, 77.37, 117.16, 134.46, 155.93.

  • 2
  • [ 26690-80-2 ]
  • [ 70122-89-3 ]
  • [ 441752-75-6 ]
YieldReaction ConditionsOperation in experiment
97.9% With tetrakis(triphenylphosphine) palladium(0) In tetrahydrofuran at 0 - 70℃; for 5h; Inert atmosphere; 2.3 (3) Step 3 Synthesis of compound 1-IM10 Add compound 1-IM7 (1.6g, 7.94mmol), tetratriphenylphosphine palladium (0.92g, 0.79mmol) into a 50mL double-necked flask, replace with nitrogen, add 20mL deoxytoluene, at 0°C , slowly add the compound 1-IM9 (1.51g, 9.52mmol), heated to 70 °C for 5 hours. After the reaction was completed, toluene was distilled off under reduced pressure, and the resulting crude product was separated and purified through a silica gel chromatography column to obtain a yellow oily liquid compound 1-IM10. Yield 97.9%;
97.9% With tetrakis(triphenylphosphine) palladium(0) In toluene at 0 - 70℃; for 5h; Inert atmosphere; General procedure B General procedure: (for the synthesis of compounds 5a-5d)Allyl tert-butyl carbonate (1.51 g, 9.52 mmol) was slowly added to asolution of tetrakistriphenylphosphane Pd (0) (0.92 g, 0.79 mmol) and tert-butyl carbamate derivatives (7.94 mmol) in toluene (20 mL) at 0 °C under nitrogen protection. After the addition was complete, the mixture was heated at 70 °C for 5 h. After it was fully reacted, the mixture was concentrated under vacuum. The residue was purified by column chromatography to afford the product.
  • 3
  • [ 441752-75-6 ]
  • [ 947664-36-0 ]
YieldReaction ConditionsOperation in experiment
Multi-step reaction with 2 steps 1.1: 9-borabicyclo[3.3.1]nonane dimer / tetrahydrofuran / 3 h / 0 - 65 °C / Inert atmosphere 1.2: 1 h / 0 °C / Inert atmosphere 2.1: hydrogenchloride / dichloromethane; 1,4-dioxane / 0.5 h / 25 °C / Inert atmosphere
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