Lithium Hydroxide → 74754-55-5

HRID 2201606Notes

Reaction equation

HRID 2201606 reaction equation
[N+:1]([O:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][C:10]([O:12]CC)=[O:11])([O-:3])=[O:2].[OH-].[Li+]>CO.C1COCC1.O>[N+:1]([O:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][C:10]([OH:12])=[O:11])([O-:3])=[O:2]

Participants

5

Reactant 2

HCID 3939Lithium HydroxideHCID 71618662HCID 71618662, compound

Product 1

HCID 2309071374754-55-5

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 21899815MeOH tetrahydrofuranSolvent

Conditions

Temperature
50 °C

Procedure

19.1 mmol Ethyl 6-nitrooxy-hexanoate were dissolved in 222 ml Methanol/THF 1:1. 37.5 ml 1M Lithiumhydroxide in Water were added to the reaction and the cloudy solution was heated for 18 hours at 50° C. After cooling to room temperature the solution was concentrated in vacuo. The pH level of the solution was brought down to 1 with HCl 25% and extracted two times with TMBE. The organic phases were combined, washed with brine, dried over Na2SO4 and the solvent was removed in vacuo leaving 3.43 g.

Workup

  1. temperatureAfter cooling to room temperature the solution
  2. concentrationwas concentrated in vacuo
  3. extractionextracted two times with TMBE
  4. washwashed with brine
  5. dry with materialdried over Na2SO4
  6. customthe solvent was removed in vacuo
  7. customleaving 3.43 g

Sources & evidence

ORD record
ord-53a85759e6c5401abbab8541ddcd2e5a
Source dataset
uspto-grants-2016_06
Patent number
US09365489B2

Reaction notes

Loading…