Hexamethyldisilazane → HCID 58422988, compound

HRID 2193856Notes

Reaction equation

HRID 2193856 reaction equation
C([O:3][P:4]([CH2:9][CH2:10][CH2:11][C:12]1[NH:16][C:15]2[CH:17]=[C:18]([Cl:33])[C:19]([C:21]3[CH:26]=[CH:25][C:24]([C:27]4[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=4)=[CH:23][CH:22]=3)=[CH:20][C:14]=2[N:13]=1)(=[O:8])[O:5]CC)C.C[Si](N[Si](C)(C)C)(C)C.Br[Si](C)(C)C>C(Cl)Cl>[C:24]1([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[CH:23]=[CH:22][C:21]([C:19]2[C:18]([Cl:33])=[CH:17][C:15]3[NH:16][C:12]([CH2:11][CH2:10][CH2:9][P:4](=[O:3])([OH:8])[OH:5])=[N:13][C:14]=3[CH:20]=2)=[CH:26][CH:25]=1

Participants

5

Reactant 3

HCID 13838HexamethyldisilazaneHCID 76113BromotrimethylsilaneHCID 86657370HCID 86657370, compound

Product 1

HCID 58422988HCID 58422988, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

To a solution of compound 25-1 (196 mg, 0.41 mmol) in 8 mL of CH2Cl2 was added hexamethyldisilizane (2 mL), followed by bromo trimethylsilane (0.54 mL, 4.1 mmol). The reaction was stirred for 18 h at ambient temperature. The organic solvent was removed in vacuo, followed by the addition of H2O (2 mL). The crude product was sonicated and yielded a grey powder. The product was collected by vacuum filtration and washed three times with H2O and two times with MeOH. The product was dried in vacuo to give title compound 25-2 as a grey solid.

Workup

  1. customThe organic solvent was removed in vacuo
  2. additionfollowed by the addition of H2O (2 mL)
  3. customThe crude product was sonicated
  4. customyielded a grey powder
  5. filtrationThe product was collected by vacuum filtration
  6. washwashed three times with H2O and two times with MeOH
  7. customThe product was dried in vacuo

Sources & evidence

ORD record
ord-8c6ce064dfe34e5796a1b1220e71edc9
Source dataset
uspto-grants-2012_12
Patent number
US08329914B2

Reaction notes

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