Toluene → HCID 68576839, compound

HRID 656471Notes

Reaction equation

HRID 656471 reaction equation
[CH2:1]([N:8]1[CH2:12][CH2:11][C:10]2([CH2:17][CH2:16][CH2:15][N:14]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[C:13]2=O)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:26]1(C)C=CC=CC=1>N1C=CC=CC=1.C1([Ti](C2C=CC=C2)(C)C)C=CC=C1>[CH2:1]([N:8]1[CH2:12][CH2:11][C:10]2([CH2:17][CH2:16][CH2:15][N:14]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[C:13]2=[CH2:26])[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Participants

5

Reactant 2

HCID 1140TolueneHCID 68575456HCID 68575456, compound

Product 1

HCID 68576839HCID 68576839, compound

Reagents, catalysts & solvents 2

HCID 178477792HCID 178477792, compoundCatalystHCID 1049PyridineSolvent

Conditions

Temperature
70 °C

Procedure

8.7 mmol of tert-butyl 2-benzyl-6-oxo-2,7-diazaspiro[4.5]decane-7-carboxylate are dissolved in a mixture of 75 ml of toluene and 0.75 ml of pyridine. The solution is admixed with 10.0 mmol of bis(cyclopentadienyl)dimethyltitanium [1271-66-5] and heated at 70° C. for 20 hours. The reaction solution is evaporated and the residue is taken up in pentane. The mixture is filtered over Hyflo and the filtrate is evaporated. From the residue the title compound is identified by means of flash chromatography (SiO2 60 F) on the basis of the Rf value.

Workup

  1. customThe reaction solution is evaporated
  2. filtrationThe mixture is filtered over Hyflo
  3. customthe filtrate is evaporated

Sources & evidence

ORD record
ord-2185e68039ff4ee38fd5a8b41360a0a3
Source dataset
uspto-grants-2011_12
Patent number
US08071773B2

Reaction notes

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