Sulfamic Acid → HCID 21841490, compound

HRID 1739564Notes

Reaction equation

HRID 1739564 reaction equation
[CH:1]([N:4]([CH:25]([CH3:27])[CH3:26])[C:5](=[O:24])[CH2:6][O:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]2[C:19]([Cl:20])=[CH:18][C:17]([CH:21]=[O:22])=[CH:16][C:15]=2[Cl:23])=[CH:10][CH:9]=1)([CH3:3])[CH3:2].[O:28]1CCCC1.O.Cl([O-])=O.[Na+].NS(O)(=O)=O>C(OCC)(=O)C.O>[CH:25]([N:4]([CH:1]([CH3:3])[CH3:2])[C:5](=[O:24])[CH2:6][O:7][C:8]1[CH:9]=[CH:10][C:11]([C:14]2[C:19]([Cl:20])=[CH:18][C:17]([C:21]([OH:28])=[O:22])=[CH:16][C:15]=2[Cl:23])=[CH:12][CH:13]=1)([CH3:27])[CH3:26]

Participants

7

Reactant 4

HCID 5987Sulfamic AcidHCID 8028TetrahydrofuranHCID 18944501HCID 18944501, compoundHCID 22664591HCID 22664591, compound

Product 1

HCID 21841490HCID 21841490, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 8857Ethyl AcetateSolvent

Procedure

124 mg of the product of Stage E were mixed with 2 ml of tetrahydrofuran, 3.5 ml of water, 98 mg of sodium chlorite monohydrate and 87 mg of amidosulfonic acid and the mixture was stirred for 90 minutes at ambient temperature and evaporated under reduced pressure to obtain a residue which was obtained which is taken up in ethyl acetate. The organic phase was washed with IN sodium hydroxide, dried over magnesium sulfate and evaporated under reduced pressure to obtain 97.8 mg of the expected product with a Rf=0.26 (cyclohexane/ethyl acetate 8/2).

Workup

  1. customevaporated under reduced pressure
  2. customto obtain a residue which
  3. customwas obtained which
  4. washThe organic phase was washed with IN sodium hydroxide
  5. dry with materialdried over magnesium sulfate
  6. customevaporated under reduced pressure

Sources & evidence

ORD record
ord-06dd83bea8814e56a6ea1169232c6776
Source dataset
uspto-grants-1999_10
Patent number
US05965763

Reaction notes

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