Water → HCID 19364621, compound

HRID 1740707Notes

Reaction equation

HRID 1740707 reaction equation
[H-].[Al+3].[Li+].[H-].[H-].[H-].[Si:7]([O:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][C:21]#[N:22])([C:10]([CH3:13])([CH3:12])[CH3:11])([CH3:9])[CH3:8].O>CCOCC>[NH2:22][CH2:21][CH2:20][CH2:19][CH2:18][CH2:17][CH2:16][CH2:15][O:14][Si:7]([C:10]([CH3:13])([CH3:12])[CH3:11])([CH3:9])[CH3:8]

Participants

5

Reactant 3

HCID 962WaterHCID 19364626HCID 19364626, compoundHCID 21226445Aluminium lithium hydride

Product 1

HCID 19364621HCID 19364621, compound

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent2×

Procedure

To a solution of lithium aluminium hydride (600 mg, Aldrich) in ether (50 mL) was added dropwise the product (3.8 g) from Example 4 in ether (50 mL). After 1-3 h, the mixture was poured into water and stirred for 30 min. The insoluble aluminium hydroxide was filtered through a celite pad, and the aqueous layer was extracted with ether three times. The ether extracts were washed with brine solution, dried and concentrated. The crude product was distilled at 0.25 Torr and 82° C. High resolution mass spectrum for C13 H31 O N Si: calculated 245.2175, found 245.2159.

Workup

  1. filtrationThe insoluble aluminium hydroxide was filtered through a celite pad
  2. extractionthe aqueous layer was extracted with ether three times
  3. washThe ether extracts were washed with brine solution
  4. customdried
  5. concentrationconcentrated
  6. distillationThe crude product was distilled at 0.25 Torr and 82° C

Sources & evidence

ORD record
ord-6fe0718f6728442c8e53e1290bfec2ba
Source dataset
uspto-grants-1999_10
Patent number
US05972349

Reaction notes

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