Water → HCID 69093550, compound

HRID 1624870Notes

Reaction equation

HRID 1624870 reaction equation
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:8](=[CH:9][C:10]=1[O:11][CH3:12])[CH:7]([NH:13][C:14](=O)OCC)[CH2:6]2.[H-].[H-].[H-].[H-].[Li+].[Al+3].O.[OH-].[Na+]>C1COCC1>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:8](=[CH:9][C:10]=1[O:11][CH3:12])[CH:7]([NH:13][CH3:14])[CH2:6]2

Participants

6

Reactant 4

HCID 962Water2×HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 86715999HCID 86715999, compound

Product 1

HCID 69093550HCID 69093550, compoundYield 93.5%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent2×

Procedure

3.2 g of the compound obtained in Step 2 dissolved in 30 mL of THF are added to a suspension of 0.9 g of LiAlH4 in 20 mL of THF. Refluxing is carried out for 1 hour 30 minutes, then hydrolysing using 0.6 ml of water and 0.5 mL of 20% sodium hydroxide solution and, finally, 2.3 mL of water. The mineral salts are then filtered off, rinsed with THF and then the filtrate obtained is evaporated to dryness. 2.3 g of the expected compound are obtained.

Workup

  1. temperatureRefluxing
  2. filtrationThe mineral salts are then filtered off
  3. washrinsed with THF
  4. customthe filtrate obtained
  5. customis evaporated to dryness

Sources & evidence

ORD record
ord-52e54fc060da414292aee9f209426187
Source dataset
uspto-grants-2014_07
Patent number
US08779123B2

Reaction notes

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