Sodium hydrosulfide → HCID 178499044, compound

HRID 477530Notes

Reaction equation

HRID 477530 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]=[C:4]([CH:15]([CH3:17])[CH3:16])[CH:3]=1.[SH-:18].[Na+]>O>[CH:15]([C:4]1[CH:3]=[C:2]([SH:18])[N:7]2[N:8]=[C:9]([C:11]([O:13][CH3:14])=[O:12])[N:10]=[C:6]2[N:5]=1)([CH3:17])[CH3:16]

Participants

4

Reactant 2

HCID 28015Sodium hydrosulfideHCID 1676769199951-44-7

Product 1

HCID 178499044HCID 178499044, compoundYield 90.8%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
0 °C

Procedure

The product obtained in Step 2 (40 g) was added at 0° C. to a solution of sodium hydrosulfide (40 g) in one liter of water with stiring under a nitrogen stream. The mixture was stirred at 0° C. for one hour, then at room temperature for three hours, and the resulting yellow solution was washed with 200 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 100 ml of ethanol, affording 36 g of the objective compound as faint yellow crystals.

Workup

  1. waitat room temperature for three hours
  2. washthe resulting yellow solution was washed with 200 ml of ethyl acetate
  3. filtrationthe formed crystals were collected by filtration
  4. washwashed with 100 ml of ethanol

Sources & evidence

ORD record
ord-19b784f30ccf444d8f16088a5716e50c
Source dataset
uspto-grants-1989_12
Patent number
US04888332

Reaction notes

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