Cyclohexene → HCID 69957540, compound

HRID 394453Notes

Reaction equation

HRID 394453 reaction equation
C([N:8]1[CH2:14][CH2:13][NH:12][CH:11]([CH3:15])[C:10]2[C:16](=[O:21])[N:17]([CH3:20])[N:18]=[CH:19][C:9]1=2)C1C=CC=CC=1.C1CCCCC=1>[Pd].C(O)C>[CH3:15][CH:11]1[NH:12][CH2:13][CH2:14][NH:8][C:9]2[CH:19]=[N:18][N:17]([CH3:20])[C:16](=[O:21])[C:10]1=2

Participants

5

Reactant 2

HCID 8079CyclohexeneHCID 18176458HCID 18176458, compound

Product 1

HCID 69957540HCID 69957540, compound

Reagents, catalysts & solvents 2

HCID 23938PalladiumCatalystHCID 702EthanolSolvent

Procedure

0.38 g (2 mmol) of 1-benzyl-5,7-dimethyl-2,3,4,5-tetrahydro-6(7H)-pyridazino[4,5-b][1,5]diazepinone, 10 ml of abs. ethanol, 2 ml of cyclohexene and 0.20 g of Pd/C are warmed for 2 hours at 80° C. After cooling the mixture is filtered. The filtrate is evaporated and the residue is taken up in 10 ml of water, then it is shaken with 4×10 ml of ethyl acetate. The ethyl acetate phase is dried with anhydrous sodium sulphate and evaporated. The crystalline material obtained is recrystallized from 2 ml of ethyl acetate.

Workup

  1. temperatureAfter cooling the mixture
  2. filtrationis filtered
  3. customThe filtrate is evaporated
  4. dry with materialThe ethyl acetate phase is dried with anhydrous sodium sulphate
  5. customevaporated
  6. customThe crystalline material obtained
  7. customis recrystallized from 2 ml of ethyl acetate

Sources & evidence

ORD record
ord-3dadb5ed108a4c96bca72b56fe02928c
Source dataset
uspto-grants-2003_08
Patent number
US06602865B1

Reaction notes

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