Sodium hydrosulfide → HCID 178499621, compound

HRID 477522Notes

Reaction equation

HRID 477522 reaction equation
Cl[C:2]1[N:7]2[N:8]=[C:9]([CH2:11][C:12]([O:14][CH3:15])=[O:13])[N:10]=[C:6]2[N:5]=[C:4]([CH3:16])[CH:3]=1.[SH-:17].[Na+]>O>[SH:17][C:2]1[N:7]2[N:8]=[C:9]([CH2:11][C:12]([O:14][CH3:15])=[O:13])[N:10]=[C:6]2[N:5]=[C:4]([CH3:16])[CH:3]=1

Participants

4

Reactant 2

HCID 28015Sodium hydrosulfideHCID 13562763HCID 13562763, compound

Product 1

HCID 178499621HCID 178499621, compoundYield 72.7%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

The product obtained in Step 4 (2 g) and sodium hydrosulfide (1.22 g) were dissolved in 35 ml of water, the solution was stirred at room temperature for 1.5 hours under a nitrogen stream, and the insoluble matters were filtered off. The filtrate was cooled to 0° C., its pH was lowered to 1-2 with 6N hydrochloric acid, the slurry was stirred at that temperature for 30 minutes, and the crystals thus formed were collected by filtration, washed with 30 ml of water and dried, affording 1.44 g of the objective compound.

Workup

  1. filtrationthe insoluble matters were filtered off
  2. temperatureThe filtrate was cooled to 0° C.
  3. stirringthe slurry was stirred at that temperature for 30 minutes
  4. customthe crystals thus formed
  5. filtrationwere collected by filtration
  6. washwashed with 30 ml of water
  7. customdried

Sources & evidence

ORD record
ord-0aab338426834364b65ed74e06356a54
Source dataset
uspto-grants-1989_12
Patent number
US04888332

Reaction notes

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