Ammonium Chloride → HCID 15865176, compound

HRID 2216719Notes

Reaction equation

HRID 2216719 reaction equation
[CH3:1][C:2]1[CH:3]=[CH:4][C:5](=[C:7]([CH3:9])[CH3:8])[CH:6]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].[NH4+].[Cl-]>CCOCC>[CH:7]([C:5]1[CH:6]=[C:2]([CH3:1])[CH2:3][CH:4]=1)([CH3:9])[CH3:8]

Participants

5

Reactant 3

HCID 25517Ammonium ChlorideHCID 143632822,6,6-TrimethylfulveneHCID 21226445Aluminium lithium hydride

Product 1

HCID 15865176HCID 15865176, compound

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent2×

Procedure

A solution of 24 g (0.2 mol) of 3,6,6-trimethylfulvene in 100 mL of ether was added at 78° C. under argon atmosphere to a solution of 7.59 g (0.2 mol) of lithium aluminium hydride in 200 mL of ether. The reaction mixture was allowed to warm to room temperature, stirred for 2 h and then treated with a 10% aq. solution of NH4Cl. The organic phase was collected, washed with water, dried with MgSO4 and concentrated. The residue was distilled at 63° C./50 mmHg. Yield 15.88 g (65%).The desired title compound was characterized by 1H-NR

Workup

  1. customThe organic phase was collected
  2. washwashed with water
  3. dry with materialdried with MgSO4
  4. concentrationconcentrated
  5. distillationThe residue was distilled at 63° C./50 mmHg

Sources & evidence

ORD record
ord-400c184bd9194e1fb08df2c41f9eb506
Source dataset
uspto-grants-2006_09
Patent number
US07112638B2

Reaction notes

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