Sulfamic Acid → HCID 71008235, compound

HRID 877020Notes

Reaction equation

HRID 877020 reaction equation
[CH3:1][N:2]1[C:7]2[S:8][C:9]([CH3:14])=[C:10]([CH2:11][CH:12]=[O:13])[C:6]=2[C:5](=[O:15])[N:4]([CH3:16])[C:3]1=[O:17].S(=O)(=O)([OH:20])N.Cl([O-])=O.[Na+]>CC(C)=O.O>[CH3:1][N:2]1[C:7]2[S:8][C:9]([CH3:14])=[C:10]([CH2:11][C:12]([OH:20])=[O:13])[C:6]=2[C:5](=[O:15])[N:4]([CH3:16])[C:3]1=[O:17]

Participants

6

Reactant 3

HCID 5987Sulfamic AcidHCID 23668197Sodium ChloriteHCID 89183467HCID 89183467, compound

Product 1

HCID 71008235HCID 71008235, compound

Reagents, catalysts & solvents 2

HCID 180AcetoneSolventHCID 962WaterSolvent

Procedure

To a solution of Step 7 intermediate (900 mg, 3.57 mmol) and sulphamic acid (693 mg, 7.142 mmol) in acetone (17.8 ml) was added sodium chlorite (484 mg, 5.357 mmol) in water (5.35 ml) and reaction mixture was stirred for 2 h. The solvent was evaporated, diluted with water and acidified with 1N HCl. Solid obtained was filtered and dried to give 375 mg of title compound as a white solid. 1H NMR (300 MHz, DMSO-d6) δ 2.30 (s, 3H), 3.20 (s, 3H), 3.42 (s, 3H), 3.80 (s, 2H), 12.19 (br s, 1H); MS (m/z) 249.10 (M+H)+.

Workup

  1. customThe solvent was evaporated
  2. additiondiluted with water
  3. customSolid obtained
  4. filtrationwas filtered
  5. customdried

Sources & evidence

ORD record
ord-1b5286c075a04dd3979699ba0098e6cb
Source dataset
uspto-grants-2015_03
Patent number
US08987278B2

Reaction notes

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