Methanol → HCID 14519823, compound

HRID 1084780Notes

Reaction equation

HRID 1084780 reaction equation
[Li].[N:2]([N:4]([C:8]([CH3:11])([CH3:10])[CH3:9])[CH2:5][CH2:6][OH:7])=O.O1CCCC1.CO>O>[C:8]([N:4]([CH2:5][CH2:6][OH:7])[NH2:2])([CH3:11])([CH3:10])[CH3:9]

Participants

6

Reactant 4

HCID 887MethanolHCID 8028TetrahydrofuranHCID 3028194Lithium2×HCID 14519822HCID 14519822, compound

Product 1

HCID 14519823HCID 14519823, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
60 °C

Procedure

A total of 12.2 g of lithium alanate are added in portions to a mixture of 23 g of N-nitroso-tert.-butyl-(2-hydroxy-ethyl)amine and 200 ml of anhydrous tetrahydrofuran at 60° C. When the addition has ended, the mixture is heated at 60° C. for a further hour and cooled in an ice bath and the excess lithium alanate is hydrolysed by careful dropwise addition of methanol and then water. The solids are removed by filtration with suction and the filtrate is concentrated. A colourless oil (14 g) remains and is subsequently used without further purification.

Workup

  1. additionWhen the addition
  2. temperaturecooled in an ice bath
  3. customThe solids are removed by filtration with suction
  4. concentrationthe filtrate is concentrated
  5. customis subsequently used without further purification

Sources & evidence

ORD record
ord-c136b7148e92436e96f06efab1f784ef
Source dataset
uspto-grants-1991_04
Patent number
US05006540

Reaction notes

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