Sulfamic Acid → HCID 66593056, compound

HRID 1091827Notes

Reaction equation

HRID 1091827 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-6406144434b241408aa454140d7f48ea
Source dataset
uspto-grants-2012_03
Patent number
US08129401B2

Reaction notes

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