Sodium sulfide nonahydrate → HCID 68750257, compound

HRID 624296Notes

Reaction equation

HRID 624296 reaction equation
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([C:10]2[CH2:15][CH2:14][CH:13]([NH:16][C:17](=[O:23])[O:18][C:19]([CH3:22])([CH3:21])[CH3:20])[CH2:12][CH:11]=2)=[CH:6][CH:5]=1)([O-])=O.O.O.O.O.O.O.O.O.O.[S-2].[Na+].[Na+]>C(O)C.O>[NH2:1][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[CH2:15][CH2:14][CH:13]([NH:16][C:17](=[O:23])[O:18][C:19]([CH3:21])([CH3:20])[CH3:22])[CH2:12][CH:11]=2)=[CH:6][CH:5]=1

Participants

5

Reactant 2

HCID 73972Sodium sulfide nonahydrateHCID 68753439HCID 68753439, compound

Product 1

HCID 68750257HCID 68750257, compound

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 962WaterSolvent

Conditions

Temperature
80 °C

Procedure

tert-Butyl 4-(4-nitrophenyl)cyclohex-3-enylcarbamate (2.55 g, 8.01 mmol) was suspended in ethanol (30 ml) followed by addition of sodium sulfide, nonahydrate (10.37 ml, 80 mmol) dissolved in water (30 ml). The mixture was heated to 80° C. for 1.5 h and extracted with dichloromethane; the organic layers were combined, dried over magnesium sulfate, filtered and concentrated to give the title compound.

Workup

  1. extractionextracted with dichloromethane
  2. dry with materialdried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated

Sources & evidence

ORD record
ord-3adf704333a0435590c7279bb5931b9d
Source dataset
uspto-grants-2016_04
Patent number
US09302989B2

Reaction notes

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