Bromotrimethylsilane → HCID 9905894, compound

HRID 1358206Notes

Reaction equation

HRID 1358206 reaction equation
Br[Si](C)(C)C.C([O:8][P:9]([C:14]1[C:15](=[O:29])[NH:16][C:17]2[C:22]([CH:23]=1)=[CH:21][C:20]([S:24](=[O:27])(=[O:26])[NH2:25])=[C:19]([Cl:28])[CH:18]=2)(=[O:13])[O:10]CC)C>C(#N)C>[Cl:28][C:19]1[CH:18]=[C:17]2[C:22]([CH:23]=[C:14]([P:9](=[O:8])([OH:13])[OH:10])[C:15](=[O:29])[NH:16]2)=[CH:21][C:20]=1[S:24](=[O:26])(=[O:27])[NH2:25]

Participants

4

Reactant 2

HCID 76113BromotrimethylsilaneHCID 88064075HCID 88064075, compound

Product 1

HCID 9905894HCID 9905894, compound

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Procedure

3.33 ml (25.3 mmol) of bromotrimethylsilane are added to a suspension of the compound obtained in Step F (1.0 g, 2.53 mmol) in 30 ml of anhydrous acetonitrile. The batch is stirred at reflux for 1 hour and evaporated to dryness. The residue is dried in vacuo and is taken up in methanol. The suspension is stirred for 30 minutes, becoming thicker and thicker. After filtering off the white precipitate and rinsing with a little methanol and then ether, the title product is obtained.

Workup

  1. temperatureat reflux for 1 hour
  2. customevaporated to dryness
  3. customThe residue is dried in vacuo
  4. stirringThe suspension is stirred for 30 minutes
  5. filtrationAfter filtering off the white precipitate
  6. washrinsing with a little methanol

Sources & evidence

ORD record
ord-1d1ad044d3134759b44a7e036ad0f5a1
Source dataset
uspto-grants-2003_07
Patent number
US06596709B1

Reaction notes

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