Water → HCID 87347349, compound

HRID 1015670Notes

Reaction equation

HRID 1015670 reaction equation
[CH2:1]([CH:3]1[O:5][CH2:4]1)Cl.O.[CH2:7]([CH:9]([CH2:20][CH2:21][CH2:22][CH3:23])[CH2:10][NH:11][CH2:12][CH:13]([CH2:18][CH3:19])[CH2:14][CH2:15][CH2:16][CH3:17])[CH3:8]>>[CH2:18]([CH:13]([CH2:14][CH2:15][CH2:16][CH3:17])[CH2:12][N:11]([CH2:1][CH:3]1[CH2:4][O:5]1)[CH2:10][CH:9]([CH2:7][CH3:8])[CH2:20][CH2:21][CH2:22][CH3:23])[CH3:19]

Participants

4

Reactant 3

HCID 962WaterHCID 7791Bis(2-ethylhexyl)amineHCID 7835Epichlorohydrin

Product 1

HCID 87347349HCID 87347349, compound

Procedure

A mixture of epichlorohydrin (111 g, 1.2 mol), and water (0.27 g, 0.015 mol) was vigorously stirred at room temperature. Bis(2-ethylhexyl)amine (241.4 g, 1.0 mol) was added slowly by an addition funnel. The mixture was slowly heated to 70° C. and then stirred at 70° C. for 6 hours. The mixture was washed with aqueous potassium carbonate, K2CO3, (20%, 200 ml). Sodium hydroxide, NaOH, (36%, 200 ml) was added to the oil phase and the mixture was stirred at 70-90° C. for 18 hours. The phases were separated and extracted with ethyl acetate (3×100 ml). The combined extracts were washed with brine, dried over magnesium sulfate, MgSO4, and the solvent removed by rotary evaporation.

Workup

  1. temperatureThe mixture was slowly heated to 70° C.
  2. stirringstirred at 70° C. for 6 hours
  3. washThe mixture was washed with aqueous potassium carbonate, K2CO3, (20%, 200 ml)
  4. additionSodium hydroxide, NaOH, (36%, 200 ml) was added to the oil phase
  5. stirringthe mixture was stirred at 70-90° C. for 18 hours
  6. customThe phases were separated
  7. extractionextracted with ethyl acetate (3×100 ml)
  8. washThe combined extracts were washed with brine
  9. dry with materialdried over magnesium sulfate, MgSO4
  10. customthe solvent removed by rotary evaporation

Sources & evidence

ORD record
ord-ffe7907d024e4a9ea6577d8de9e4f684
Source dataset
uspto-grants-2011_07
Patent number
US07985795B2

Reaction notes

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