Water → HCID 15078701, compound

HRID 2050524Notes

Reaction equation

HRID 2050524 reaction equation
Cl[C:2]1[C:11]([C:12]#[N:13])=[C:10]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=[CH:9]2)[N:3]=1.C(=O)([O-])[O-].[K+].[K+].Cl.[CH3:21][O:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=1[N:29]1[CH2:34][CH2:33]C[CH2:31][CH2:30]1.O.C[N:37](C)C=O>>[C:12]([C:11]1[C:2]([N:37]2[CH2:33][CH2:34][N:29]([C:24]3[CH:25]=[CH:26][CH:27]=[CH:28][C:23]=3[O:22][CH3:21])[CH2:30][CH2:31]2)=[N:3][C:4]2[C:10]=1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=2)#[N:13]

Participants

6

Reactant 5

HCID 962WaterHCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 10261891HCID 10261891, compoundHCID 131716884HCID 131716884, compound

Product 1

HCID 15078701HCID 15078701, compoundYield 97.2%

Procedure

To a solution of 1.0 g (0.0053 mol) of 2-chloro-3-cyano-1-azaazulene in 20 ml of dimethylformamide were added 0.7 g (0.0053 mol) of anhydrous potassium carbonate and 1.2 g (0.0053 mol) of 2-methoxyphenylpiperadine hydrochloride. The reaction mixture was stirred at room temperature for 24 hours. The reaction mixture was poured into water with ice, and the precipitate was filtered and washed with water. After drying, the precipitate was recrystallized from mixture of ethyl acetate and petroleum ether to give 3.5 g of title compound (yield: 97.2%).

Workup

  1. filtrationthe precipitate was filtered
  2. washwashed with water
  3. customAfter drying
  4. customthe precipitate was recrystallized from mixture of ethyl acetate and petroleum ether

Sources & evidence

ORD record
ord-77dc0848f4154ffea26c28aab1b8ee19
Source dataset
uspto-grants-1991_05
Patent number
US05013736

Reaction notes

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