Aluminium lithium hydride → HCID 21919289, compound

HRID 898690Notes

Reaction equation

HRID 898690 reaction equation
[H-].[H-].[H-].[H-].[Li+].[Al+3].C([O:9][C:10]([C:12]1[N:13]=[N:14][C:15]([O:21][CH2:22][CH3:23])=[CH:16][C:17]=1[O:18][CH2:19][CH3:20])=O)C>C1COCC1>[CH2:19]([O:18][C:17]1[CH:16]=[C:15]([O:21][CH2:22][CH3:23])[N:14]=[N:13][C:12]=1[CH2:10][OH:9])[CH3:20]

Participants

4

Reactant 2

HCID 21226445Aluminium lithium hydrideHCID 58661538Ethyl 4,6-diethoxypyridazine-3-carboxylate

Product 1

HCID 21919289HCID 21919289, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Conditions

Temperature
0 °C

Procedure

LiAlH4 (1N solution in THF, 1 mL) is added to a stirred solution of 4,6-diethoxy-pyridazine-3-carboxylic acid ethyl ester (213 mg, 0.8 mmol) in THF (8 mL), cooled to 0° C. The solution is stirred at 0° C. for 3 hours. Excess Na2SO4.10H2O is then added and the mixture is stirred at room temperature for 45 minutes. The solid is filtered and washed with EtOAc. Evaporation of the filtrate in vacuo provides a light yellow oil. This alcohol used in the next step without further purification. LC-MS (M+1) 199.2.

Workup

  1. stirringthe mixture is stirred at room temperature for 45 minutes
  2. filtrationThe solid is filtered
  3. washwashed with EtOAc
  4. customEvaporation of the filtrate in vacuo
  5. customprovides a light yellow oil
  6. customThis alcohol used in the next step without further purification

Sources & evidence

ORD record
ord-8a8ecf8fb0d744dd812bfb818d274000
Source dataset
uspto-grants-2008_04
Patent number
US07351826B2

Reaction notes

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