Bromotrimethylsilane → HCID 9951841, compound

HRID 1018909Notes

Reaction equation

HRID 1018909 reaction equation
Br[Si](C)(C)C.C([O:8][P:9]([C:14]1[C:15](=[O:32])[NH:16][C:17]2[C:22]([CH:23]=1)=[CH:21][C:20]([S:24]([NH:27][CH2:28][CH2:29][CH3:30])(=[O:26])=[O:25])=[C:19]([Cl:31])[CH:18]=2)(=[O:13])[O:10]CC)C>C(#N)C>[Cl:31][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:32])[NH:16]2)=[CH:21][C:20]=1[S:24]([NH:27][CH2:28][CH2:29][CH3:30])(=[O:25])=[O:26]

Participants

4

Reactant 2

HCID 76113BromotrimethylsilaneHCID 15895895HCID 15895895, compound

Product 1

HCID 9951841HCID 9951841, compound

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Procedure

25.3 mmol of bromotrimethylsilane are added to a suspension of the compound obtained in Example 1 (2.53 mmol) in 30 ml of anhydrous acetonitrile. Stirring is carried out at reflux for 1 hour, followed by evaporation to dryness. The residue is dried in vacuo and taken up in methanol. The suspension is stirred for 30 minutes and becomes increasingly thick. The precipitate is filtered off and rinsed with a small amount of methanol to obtain the title product.

Workup

  1. temperatureat reflux for 1 hour
  2. customfollowed by evaporation to dryness
  3. customThe residue is dried in vacuo
  4. stirringThe suspension is stirred for 30 minutes
  5. temperaturebecomes increasingly thick
  6. filtrationThe precipitate is filtered off
  7. washrinsed with a small amount of methanol

Sources & evidence

ORD record
ord-a21e14db46374a8488cab137bf86aaea
Source dataset
uspto-grants-2002_11
Patent number
US06486143B2

Reaction notes

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