Ethanamine, 2,2,2-trifluoro- → HCID 123649658, compound

HRID 2273158Notes

Reaction equation

HRID 2273158 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].[F:15][C:16]([F:20])([F:19])[CH2:17][NH2:18]>CCCCCC>[C:11]([N:3]1[CH:4]=[CH:5][N:6]([C:7]([CH3:10])([CH3:9])[CH3:8])[SiH:2]1[NH:18][CH2:17][C:16]([F:20])([F:19])[F:15])([CH3:14])([CH3:13])[CH3:12]

Participants

4

Reactant 2

HCID 9773Ethanamine, 2,2,2-trifluoro-HCID 713346111,3-Di-tert-butyl-2-chloro-2,3-dihydro-1H-1,3,2-diazasilole

Product 1

HCID 123649658HCID 123649658, compoundYield 66%

Reagents, catalysts & solvents 1

HCID 8058HexaneSolvent

Procedure

In an argon atmosphere, 5.63 g (24.2 mmol) of Si(tBuNCHCHNtBu)(H)Cl was dissolved in 20 mL of hexane and after adding 5.38 g (54.3 mmol) of 2,2,2-trifluoroethylamine, the mixture was stirred at room temperature for 15 hours. 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./4.7×102 Pa) to obtain 1,3-di-tert-butyl-2-(2,2,2-trifluoroethyl)amino-1,3-diaza-2-silacyclopent-4-ene (Si(tBuNCHCHNtBu)(H)NHCH2CF3) as a pale yellow liquid (yielded amount: 4.74 g, yield: 66%).

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./4.7×102 Pa)
  5. customto obtain

Sources & evidence

ORD record
ord-8c95413d4d254f4592f1416e89d2a98e
Source dataset
uspto-grants-2015_09
Patent number
US09120825B2

Reaction notes

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