Hydrogen Bromide → HCID 86700699, compound

HRID 2408350Notes

Reaction equation

HRID 2408350 reaction equation
C(OC(=O)[NH:5][C:6]([CH3:11])([CH3:10])[CH2:7][CH2:8][NH2:9])C.[BrH:13]>C(O)(=O)C>[BrH:13].[BrH:13].[CH3:10][C:6]([NH2:5])([CH3:11])[CH2:7][CH2:8][NH2:9]

Participants

4

Reactant 2

HCID 260Hydrogen BromideHCID 89883778HCID 89883778, compound

Product 1

HCID 86700699HCID 86700699, compoundYield 55%

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

2.8 g of ethyl(3-amino-1,1-dimethylpropyl)carbamate are cooled with an ice bath. 9.9 mL of 33% HBr in acetic acid are added dropwise and then the mixture is refluxed with heating for 2 h. After returning to RT, the product is precipitated with Et2O, and filtered. The obtained powder is dried in the oven at 70° C. 2.34 g (yield=55%) of 3-methylbutane-1,3-diamine dihydrobromide are obtained as a white powder used as such.

Workup

  1. temperaturethe mixture is refluxed
  2. temperaturewith heating for 2 h
  3. customAfter returning to RT
  4. customthe product is precipitated with Et2O
  5. filtrationfiltered
  6. customThe obtained powder is dried in the oven at 70° C

Sources & evidence

ORD record
ord-50d3b15ddf124d78b1f6fa6b4340225b
Source dataset
uspto-grants-2014_08
Patent number
US08815853B2

Reaction notes

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