Potassium sodium tartarate → HCID 15086846, compound

HRID 1885544Notes

Reaction equation

HRID 1885544 reaction equation
[CH3:1][N:2]([CH3:26])[C:3]1[N:8]=[C:7]([CH:9]([CH3:11])[CH3:10])[C:6]([CH2:12][O:13][CH3:14])=[C:5]([C:15]2[CH:20]=[CH:19][C:18]([F:21])=[CH:17][CH:16]=2)[C:4]=1[C:22](OC)=[O:23].C(C(C(C([O-])=O)O)O)([O-])=O.[Na+].[K+]>C1(C)C=CC=CC=1.O1CCCC1.O>[CH3:26][N:2]([CH3:1])[C:3]1[N:8]=[C:7]([CH:9]([CH3:10])[CH3:11])[C:6]([CH2:12][O:13][CH3:14])=[C:5]([C:15]2[CH:16]=[CH:17][C:18]([F:21])=[CH:19][CH:20]=2)[C:4]=1[CH2:22][OH:23]

Participants

6

Reactant 2

HCID 9855836Potassium sodium tartarateHCID 19879209HCID 19879209, compound

Product 1

HCID 15086846HCID 15086846, compound

Reagents, catalysts & solvents 3

HCID 962WaterSolventHCID 1140TolueneSolventHCID 8028TetrahydrofuranSolvent

Conditions

Temperature
60 °C

Procedure

2.8 ml (9.8 mmol) of a 3.5 molar solution of sodium bis-(2-methoxyethoxy)-dihydroaluminate in toluene are added under nitrogen to a solution of 1.83 g (4.9 mmol) of the compound from Example 13 in 10 ml of dry tetrahydrofuran at 25° C. and the mixture is stirred overnight at 60° C. After cooling to 20° C., a solution of 10 g of potassium sodium tartrate in 20 ml of water is added dropwise cautiously and the mixture is extracted three times with 100 ml of ethyl acetate each time. The combined organic phases are washed once with saturated sodium chloride solution, dried over sodium sulphate and concentrated in vacuo.

Workup

  1. temperatureAfter cooling to 20° C.
  2. extractionthe mixture is extracted three times with 100 ml of ethyl acetate each time
  3. washThe combined organic phases are washed once with saturated sodium chloride solution
  4. dry with materialdried over sodium sulphate
  5. concentrationconcentrated in vacuo

Sources & evidence

ORD record
ord-7bcdd398ab1e47048c676f086b441d67
Source dataset
uspto-grants-1992_09
Patent number
US05145857

Reaction notes

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