Sodium Bicarbonate → HCID 178523112, compound

HRID 433068Notes

Reaction equation

HRID 433068 reaction equation
C[O:2][C:3]1[CH:4]=[CH:5][C:6]2[N:14]3[C:9]([CH2:10][CH2:11][CH2:12][CH2:13]3)=[C:8]([CH2:15][CH2:16][NH:17][C:18]([C:20]3[O:21][CH:22]=[CH:23][CH:24]=3)=[O:19])[C:7]=2[N:25]=1.[Cl-].[Al+3].[Cl-].[Cl-].C(=O)([O-])O.[Na+]>ClCCl>[OH:2][C:3]1[CH:4]=[CH:5][C:6]2[N:14]3[C:9]([CH2:10][CH2:11][CH2:12][CH2:13]3)=[C:8]([CH2:15][CH2:16][NH:17][C:18]([C:20]3[O:21][CH:22]=[CH:23][CH:24]=3)=[O:19])[C:7]=2[N:25]=1

Participants

5

Reactant 3

HCID 516892Sodium BicarbonateHCID 6451240Aluminum(III) ChlorideHCID 18758200HCID 18758200, compound

Product 1

HCID 178523112HCID 178523112, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

Under argon and in an anhydrous medium, 0.884 mmol of the compound obtained in Example 16 is dissolved in 16 ml of dichloromethane, and then 4.42 mmol of aluminium chloride are added. The reaction mixture is stirred at reflux for 18 hours. The reaction mixture is hydrolysed, and then neutralised with a sodium hydrogen carbonate solution. After extraction with dichloromethane, the organic phases are dried over magnesium sulphate and evaporated in vacuo. The resulting residue is washed with hexane and diethyl ether to yield the title product.

Workup

  1. temperatureat reflux for 18 hours
  2. extractionAfter extraction with dichloromethane
  3. dry with materialthe organic phases are dried over magnesium sulphate
  4. customevaporated in vacuo
  5. washThe resulting residue is washed with hexane and diethyl ether

Sources & evidence

ORD record
ord-8cae29b5cf974b959846c314f12c3e0d
Source dataset
uspto-grants-2003_12
Patent number
US06667304B2

Reaction notes

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