Diethylamine → HCID 13651231, compound

HRID 1380438Notes

Reaction equation

HRID 1380438 reaction equation
[CH2:1]([NH:3][CH2:4][CH3:5])[CH3:2].Cl[Si:7]([CH3:14])([CH3:13])[O:8][Si:9](Cl)([CH3:11])[CH3:10]>CCOCC>[CH2:1]([N:3]([Si:7]([CH3:14])([CH3:13])[O:8][Si:9]([N:3]([CH2:4][CH3:5])[CH2:1][CH3:2])([CH3:11])[CH3:10])[CH2:4][CH3:5])[CH3:2]

Participants

4

Reactant 2

HCID 8021DiethylamineHCID 75461Disiloxane, 1,3-dichloro-1,1,3,3-tetramethyl-

Product 1

HCID 13651231HCID 13651231, compound

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent

Procedure

Diethylamine, 184 g. (2.50 mole) of 400 ml. of anhydrous ether were added to a one-liter multi-necked round bottom flask equipped with reflux condenser, pressure equalizing addition funnel, thermometer and stirrer, which was maintained under a positive pressure of argon. The solution was chilled with an ice water bath to 5°-10° C. during the dropwise addition of 100 g. (0.50 mole) of 1,3-dichloro-1,1,3,3,-tetramethyldisiloxane. After addition was completed the mixture was stirred overnight at room temperature (20°-25° C.). The mixture was then filtered and the filtrate was concentrated by rotary evaporation. The resulting residue was distilled at reduced pressure and yielded 81 g. (0.29 mole; 60% theoretical) of V (b.p. 75°-80° C., 2 mm. Hg.).

Workup

  1. customequipped
  2. temperaturewith reflux condenser
  3. additionaddition funnel
  4. temperaturethermometer and stirrer, which was maintained under a positive pressure of argon
  5. temperatureThe solution was chilled with an ice water bath to 5°-10° C. during the dropwise addition of 100 g
  6. additionAfter addition
  7. filtrationThe mixture was then filtered
  8. concentrationthe filtrate was concentrated by rotary evaporation
  9. distillationThe resulting residue was distilled at reduced pressure
  10. customyielded 81 g

Sources & evidence

ORD record
ord-10555f6722e84dbd9135482a84ae0f47
Source dataset
uspto-grants-1986_04
Patent number
US04581461

Reaction notes

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