Water → HCID 19100946, compound

HRID 1975023Notes

Reaction equation

HRID 1975023 reaction equation
[CH2:1]([N:8]1[CH2:15][CH2:14][CH:13]2[CH:9]1[CH:10]([CH3:21])[N:11]([C:16](OCC)=O)[CH2:12]2)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[K+]>O1CCCC1>[CH2:1]([N:8]1[CH2:15][CH2:14][CH:13]2[CH:9]1[CH:10]([CH3:21])[N:11]([CH3:16])[CH2:12]2)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

Participants

6

Reactant 4

HCID 962Water2×HCID 14797Potassium HydroxideHCID 19100936HCID 19100936, compoundHCID 21226445Aluminium lithium hydride

Product 1

HCID 19100946HCID 19100946, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent2×

Procedure

14.4 9 (50 mm0l) of ethyl 2-benzyl-8-methyl-2,7-diazabicyclo[3.3.0)octane-7-carboxylate in 20 ml of absolute tetrahydrofuran are added dropwise to 3.8 g (0.1 mol) of lithium aluminium hydride in 100 ml of absolute tetrahydrofuran, and the mixture is subsequently refluxed overnight. The mixture is decomposed in succession with in each case 4 ml of water, 15% strength potassium hydroxide solution and water, and the inorganic salts are filtered off with suction and extracted three times by boiling with 50 ml portions of tetrahydrofuran. The organic solutions are concentrated, and the residue is distilled.

Workup

  1. filtrationthe inorganic salts are filtered off with suction
  2. extractionextracted three times
  3. concentrationThe organic solutions are concentrated
  4. distillationthe residue is distilled

Sources & evidence

ORD record
ord-ff7e4ecae3474f41aef54e7b0f11c898
Source dataset
uspto-grants-1994_02
Patent number
US05284855

Reaction notes

Loading…