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Water → HCID 22248392, compound

HRID 890082
Notes
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Reaction equation

HRID 890082 reaction equation
[C:1]([O:5][C:6]1[C:11]([C:12](OCC)=[O:13])=[CH:10][N:9]=[CH:8][N:7]=1)([CH3:4])([CH3:3])[CH3:2].[H-].C([Al+]CC(C)C)C(C)C.C(C(C(C([O-])=O)O)O)([O-])=O.[Na+].[K+].O>C1(C)C=CC=CC=1.C(OCC)(=O)C>[C:1]([O:5][C:6]1[C:11]([CH:12]=[O:13])=[CH:10][N:9]=[CH:8][N:7]=1)([CH3:4])([CH3:2])[CH3:3]
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

7

Reactant 4

HCID 962WaterHCID 9855836Potassium sodium tartarateHCID 21225700DiisobutylaluminumhydrideHCID 22248166HCID 22248166, compound

Product 1

HCID 22248392HCID 22248392, compoundYield 108.4%

Reagents, catalysts & solvents 2

HCID 1140
Toluene
Solvent
HCID 8857Ethyl AcetateSolvent

Conditions

Temperature
-78 °C

Procedure

After dissolving 976 mg of ethyl 4-tert-butoxypyrimidine-5-carboxylate in 15 ml of toluene, the solution was cooled to −78° C. 3.2 ml of diisobutylaluminium hydride (1.5 M, toluene solution) was added dropwise while stirring, and then after 30 minutes, an aqueous solution of potassium sodium (+)-tartrate was added and the mixture was stirred at room temperature. Water was added to the reaction solution and extraction was performed with ethyl acetate. The organic layer was washed with water and saturated brine in that order and dried over anhydrous magnesium sulfate, and then the solvent was distilled off under reduced pressure to obtain 0.85 g of crude 4-tert-butoxypyrimidine-5-carboxaldehyde.

Workup

  1. stirringthe mixture was stirred at room temperature
  2. washThe organic layer was washed with water and saturated brine in that order
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure

Sources & evidence

ORD record
ord-0de7dbae9e8649488024389144dd4d0c
Source dataset
uspto-grants-2006_02
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US06995144B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes