Sodium hydrosulfide → HCID 178499050, compound

HRID 973833Notes

Reaction equation

HRID 973833 reaction equation
Cl[C:2]1[N:7]2[N:8]=[C:9]([C:11]([O:13][CH3:14])=[O:12])[N:10]=[C:6]2[N:5]=[CH:4][CH:3]=1.[SH-:15].[Na+]>O>[SH:15][C:2]1[N:7]2[N:8]=[C:9]([C:11]([O:13][CH3:14])=[O:12])[N:10]=[C:6]2[N:5]=[CH:4][CH:3]=1

Participants

4

Reactant 2

HCID 28015Sodium hydrosulfideHCID 19989194HCID 19989194, compound

Product 1

HCID 178499050HCID 178499050, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

The product obtained in Step 2 was added all at once at 0° C. to a solution of sodium hydrosulfide (20 g) in 450 ml of water with stirring under a nitrogen stream. The mixture was stirred at 0° C. for one hour, then for two hours at room temperature, and the resulting yellow solution was washed with 100 ml of ethyl acetate. The aqueous layer was acidified with concentrated hydrochloric acid to pH 2.0, and the formed crystals were collected by filtration and washed with 200 ml of ethanol, affording 18 g of the objective compound as faint yellow crystals.

Workup

  1. stirringThe mixture was stirred at 0° C. for one hour
  2. washthe resulting yellow solution was washed with 100 ml of ethyl acetate
  3. filtrationthe formed crystals were collected by filtration
  4. washwashed with 200 ml of ethanol

Sources & evidence

ORD record
ord-b3f4e5e3a62a4698b190a784952e8cca
Source dataset
uspto-grants-1991_11
Patent number
US05064953

Reaction notes

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