Ammonia → HCID 12789962, compound

HRID 435193Notes

Reaction equation

HRID 435193 reaction equation
[CH3:1][Si:2]([CH3:9])([CH3:8])[NH:3][Si](C)(C)C.[S:10]1([C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[C:14](=[O:15])N1)(=[O:12])=[O:11].N.S(=O)(=O)(O)O>O.C(#N)C>[CH3:1][Si:2]([N:3]1[C:14](=[O:15])[C:16]2[C:21](=[CH:20][CH:19]=[CH:18][CH:17]=2)[S:10]1(=[O:12])=[O:11])([CH3:9])[CH3:8]

Participants

7

Reactant 4

HCID 222Ammonia2×HCID 1118Sulfuric AcidHCID 5143SaccharinHCID 13838Hexamethyldisilazane

Product 1

HCID 12789962HCID 12789962, compoundYield 102%

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 6342AcetonitrileSolvent

Procedure

2 ml (9.6 mmoles) of hexamethyldisilazane were added to a refluxing mixture of 1.83 mg (10 mmoles) of saccharin, 10 mg (0.02 mmole) of di-4-nitrophenyl N-(4-toluenesulfonyl)-phosphoramidate and 20 ml of acetonitrile under dry nitrogen and the ammonia evolved was led into water by the nitrogen stream and was titrated with 1 N sulfuric acid. The calculated amount of ammonia was evolved within 0.5 hour and the solvent and other volatile materials were removed by evaporation in a rotating film evaporator. Then, the residue was dried under vacuum to obtain 2.50 g (98%) of trimethylsilylsaccharin melting at 90°-92° C.

Workup

  1. customthe solvent and other volatile materials were removed by evaporation in a rotating film evaporator
  2. customThen, the residue was dried under vacuum

Sources & evidence

ORD record
ord-37eaa505b76a4391a3d5b28ae46c7c0c
Source dataset
uspto-grants-1983_08
Patent number
US04400509

Reaction notes

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