Iodine → HCID 18921557, compound

HRID 1289436Notes

Reaction equation

HRID 1289436 reaction equation
C([O:3][P:4]([CH:9]1[N:14]2[C:15](=[O:27])[C:16](=[O:26])[NH:17][C:18]3[CH:19]=[C:20]([C:22]([F:25])([F:24])[F:23])[CH:21]=[C:12]([C:13]=32)[CH2:11][CH2:10]1)(=[O:8])[O:5]CC)C.S(=O)(=O)(O)O.II.[I:35](O)(=O)=O>C(O)(=O)C.O>[I:35][C:21]1[C:20]([C:22]([F:25])([F:24])[F:23])=[CH:19][C:18]2[NH:17][C:16](=[O:26])[C:15](=[O:27])[N:14]3[CH:9]([P:4]([OH:5])(=[O:8])[OH:3])[CH2:10][CH2:11][C:12]=1[C:13]=23

Participants

7

Reactant 4

HCID 807IodineHCID 1118Sulfuric AcidHCID 24345Iodic acidHCID 15225059HCID 15225059, compound

Product 1

HCID 18921557HCID 18921557, compoundYield 31.7%

Reagents, catalysts & solvents 2

HCID 176Acetic AcidSolventHCID 962WaterSolvent

Conditions

Temperature
80 °C

Procedure

406 mg of 9-trifluoromethyl-2,3-dioxo-1,2,3,5,6,7-hexahydro-pyrido[1,2,3-de]quinoxaline-5-phosphonic acid diethyl ester in 2 ml of glacial acetic acid is mixed with 0.05 ml of water, 0.025 ml of concentrated sulfuric acid, 178 mg of iodine and 70 mg of iodic acid and stirred for 15 hours at 80° C. bath temperature. After concentration by evaporation, it is mixed with water and the product is suctioned off. 60 mg of 8-iodo-9-trifluoromethyl-2,3-dioxo-1,2,3,5,6,7-hexahydro-pyrido[1,2,3-de]quinoxaline-5-phosphonic acid of melting point 307° C. (with decomposition) is obtained.

Workup

  1. concentrationAfter concentration
  2. customby evaporation, it
  3. additionis mixed with water

Sources & evidence

ORD record
ord-a0bef7d63c9b42f7aaec1194f04cb15c
Source dataset
uspto-grants-1998_05
Patent number
US05750526

Reaction notes

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