Methylamine → HCID 123367279, compound

HRID 2273150Notes

Reaction equation

HRID 2273150 reaction equation
Cl[SiH:2]1[N:6]([C:7]([CH3:10])([CH3:9])[CH3:8])[CH:5]=[CH:4][N:3]1[C:11]([CH3:14])([CH3:13])[CH3:12].O1CCCC1.[CH3:20][NH2:21]>CCCCCC>[C:11]([N:3]1[CH:4]=[CH:5][N:6]([C:7]([CH3:10])([CH3:9])[CH3:8])[SiH:2]1[NH:21][CH3:20])([CH3:14])([CH3:13])[CH3:12]

Participants

5

Reactant 3

HCID 6329MethylamineHCID 8028TetrahydrofuranHCID 713346111,3-Di-tert-butyl-2-chloro-2,3-dihydro-1H-1,3,2-diazasilole

Product 1

HCID 123367279HCID 123367279, compoundYield 86%

Reagents, catalysts & solvents 1

HCID 8058HexaneSolvent

Procedure

In an argon atmosphere, 5.24 g (22.5 mmol) of Si(tBuNCHCHNtBu)(H)Cl was dissolved in 20 mL of hexane and after adding 25.0 mL (48.8 mmol) of a tetrahydrofuran solution (concentration: 1.95 mol/L) of methylamine, the mixture was stirred at room temperature for 1 hour. Insoluble matters produced were separated by filtration, and the solvent was removed by distillation from the filtrate under atmospheric pressure. The obtained residue was distilled under reduced pressure (distillation temperature: 80° C./3.8×102 Pa) to obtain 1,3-di-tert-butyl-2-methylamino-1,3-diaza-2-silacyclopent-4-ene (Si(tBuNCHCHNtBu)(H)NHMe) as a pale yellow liquid (yielded amount: 4.41 g, yield: 86%).

Workup

  1. customInsoluble matters produced
  2. customwere separated by filtration
  3. customthe solvent was removed by distillation from the filtrate under atmospheric pressure
  4. distillationThe obtained residue was distilled under reduced pressure (distillation temperature: 80° C./3.8×102 Pa)
  5. customto obtain

Sources & evidence

ORD record
ord-14115cedbefc4ad6bc5aa51d04627485
Source dataset
uspto-grants-2015_09
Patent number
US09120825B2

Reaction notes

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