HCID 18992239, compound → HCID 15337796, compound

HRID 375617Notes

Reaction equation

HRID 375617 reaction equation
[CH3:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6](=S)[N:7]3[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12][C:8]3=[N:9]2)=[CH:4][CH:3]=1>O1CCCC1.[Ni]>[CH3:1][C:2]1[CH:11]=[C:10]2[C:5]([CH2:6][N:7]3[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12][C:8]3=[N:9]2)=[CH:4][CH:3]=1

Participants

4

Reactant 1

HCID 18992239HCID 18992239, compound

Product 1

HCID 15337796HCID 15337796, compound

Reagents, catalysts & solvents 2

HCID 935NickelCatalystHCID 8028TetrahydrofuranSolvent

Procedure

To a mechanically stirred solution of 5 g of 3-methyl-7,8,9,10-tetrahydroazepino[2,1-b]quinazoline-12(6H)-thione in 150 mL of boiling tetrahydrofuran was added in small portions wet Raney nickel (W-2, Davison Chemical, Chattanooga, Tenn.). The progress of the reaction was followed by TLC. When the reaction was complete, the mixture was filtered, solids on the filter were washed thoroughly with tetrahydrofuran and the filtrate was concentrated down. The rest of the workup was identical to that described in method A.

Workup

  1. filtrationthe mixture was filtered
  2. washsolids on the filter were washed thoroughly with tetrahydrofuran
  3. concentrationthe filtrate was concentrated down

Sources & evidence

ORD record
ord-92e2953887524df6b32e2ef4598bd23f
Source dataset
uspto-grants-1996_01
Patent number
US05486512

Reaction notes

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