Iodine → HCID 10172205, compound

HRID 2217339Notes

Reaction equation

HRID 2217339 reaction equation
[CH2:1]1[CH2:12][C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:4](=O)[CH2:3][CH2:2]1.[NH2:13][C:14]([NH2:16])=[S:15].[I:17]I>O>[IH:17].[N:13]1[C:4]2[C:6]3[CH:7]=[CH:8][CH:9]=[CH:10][C:11]=3[CH2:12][CH2:1][CH2:2][C:3]=2[S:15][C:14]=1[NH2:16]

Participants

5

Reactant 3

HCID 807IodineHCID 70003BenzosuberoneHCID 2723790Thiourea

Product 1

HCID 10172205HCID 10172205, compoundYield 65%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
95 °C

Procedure

A mixture of 1-benzosuberone (1.00 mL; 6.7 mmol), thiourea (1.02 g; 13.4 mmol) and iodine (1.70 g; 6.7 mmol) were heated to 95° C. with stirring. After 20 hr., the mixture was allowed to cool to room temperature, diluted with 200 mL of water, the solid material filtered off washed twice with 25 mL of water followed by diethyl ether (3×20 mL) to provide 1.50 g of 5,6-Dihydro-4H-3-thia-1-aza-benzo[e]azulen-2-ylamine hydroiodide 17 as an off white powder.

Workup

  1. temperatureto cool to room temperature
  2. filtrationthe solid material filtered off
  3. washwashed twice with 25 mL of water

Sources & evidence

ORD record
ord-4f2dfa1211724d66ae675db8dc27cc87
Source dataset
uspto-grants-2008_08
Patent number
US07407977B2

Reaction notes

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