Sodium Carbonate → HCID 20549811, compound

HRID 2058600Notes

Reaction equation

HRID 2058600 reaction equation
Cl[CH2:2][C:3]([N:5]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[NH:9][C:8](=[O:16])[C:7]2[N:17]([CH3:21])[N:18]=[C:19]([CH3:20])[C:6]1=2)=[O:4].[NH:22]1[CH2:26][CH2:25][CH2:24][CH2:23]1.C(=O)([O-])[O-].[Na+].[Na+]>C(O)C>[CH3:21][N:17]1[C:7]2[C:8](=[O:16])[NH:9][C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=3[N:5]([C:3](=[O:4])[CH2:2][N:22]3[CH2:26][CH2:25][CH2:24][CH2:23]3)[C:6]=2[C:19]([CH3:20])=[N:18]1

Participants

5

Reactant 3

HCID 10340Sodium CarbonateHCID 31268PyrrolidineHCID 205498784-Chloroacetyl-1,3-dimethyl-1,4,9,10-tetrahydropyrazolo[4,3-b][1,5]benzodiazepin-10-one

Product 1

HCID 20549811HCID 20549811, compoundYield 92%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

2.0 g of 4-chloroacetyl-1,3-dimethyl-1,4,9,10-tetrahydropyrazolo[4,3-b][1,5]benzodiazepin-10-one, 0.55 g of pyrrolidine, 0.85 g of ground sodium carbonate and 15 ml of absolute ethanol are heated at the boil for 2 hours; the hot solution is then filtered and concentrated in vacuo. The thus-obtained residue is dissolved in ethylene chloride, and the resulting organic solution is washed at pH 7 with water and concentrated to yield 2.05 g of 1,3-dimethyl-4-(pyrrolidinoacetyl)-1,4,9,10-tetrahydropyrazolo[4,3-b][1,5]benzodiazepin-10-one, mp 114° to 116° C. (from toluene).

Workup

  1. filtrationthe hot solution is then filtered
  2. concentrationconcentrated in vacuo
  3. dissolutionThe thus-obtained residue is dissolved in ethylene chloride
  4. washthe resulting organic solution is washed at pH 7 with water
  5. concentrationconcentrated

Sources & evidence

ORD record
ord-f85ac4767d5d413b8d645337600d6500
Source dataset
uspto-grants-1982_03
Patent number
US04317823

Reaction notes

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