Sulfamic Acid → HCID 66593056, compound

HRID 548964Notes

Reaction equation

HRID 548964 reaction equation
[CH:1]([C:3]1[C:11]2[C:10]([CH3:12])=[C:9]([C:13]([O:15][CH2:16][CH3:17])=[O:14])[O:8][C:7]=2[C:6]([O:18][CH3:19])=[CH:5][CH:4]=1)=[O:2].S(=O)(=O)([OH:22])N.Cl([O-])=O.[Na+]>CC(C)=O.O>[CH2:16]([O:15][C:13]([C:9]1[O:8][C:7]2[C:6]([O:18][CH3:19])=[CH:5][CH:4]=[C:3]([C:1]([OH:22])=[O:2])[C:11]=2[C:10]=1[CH3:12])=[O:14])[CH3:17]

Participants

6

Reactant 3

HCID 5987Sulfamic AcidHCID 23668197Sodium ChloriteHCID 86636826HCID 86636826, compound

Product 1

HCID 66593056HCID 66593056, compound

Reagents, catalysts & solvents 2

HCID 180AcetoneSolventHCID 962WaterSolvent2×

Procedure

The solution of ethyl 4-formyl-7-methoxy-3-methylbenzo[b]furan-2-carboxylate (3.0 g, 11.4 mmol) in acetone (30 ml) was cooled to 10-20° C. Sulfamic acid (1.55 g, 17.1 mmol) was added at once to the reaction mixture at 10-20° C. Then solution of sodium chlorite (1.6 g, 17.1 mmol) in water (10 ml) was added dropwise at the same temp. Water (100 ml) was added to reaction mixture. Acetone was distilled off under vacuum. The solid obtained was filtered and suck dried. Yellow coloured solid (3.0 g) was obtained.

Workup

  1. distillationAcetone was distilled off under vacuum
  2. customThe solid obtained
  3. filtrationwas filtered
  4. customsuck dried
  5. customwas obtained

Sources & evidence

ORD record
ord-0383289ccc9c4a0f9c282ed7e67a996d
Source dataset
uspto-grants-2011_05
Patent number
US07943634B2

Reaction notes

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