Magnesium Hydroxide → HCID 178447305, compound

HRID 2060076Notes

Reaction equation

HRID 2060076 reaction equation
[CH3:1][CH2:2][CH2:3][CH2:4][C:5]([N:7]([C@H:26]([C:30]([OH:32])=[O:31])[CH:27]([CH3:29])[CH3:28])[CH2:8][C:9]1[CH:10]=[CH:11][C:12]([C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][C:20]=2[C:21]2[NH:22][N:23]=[N:24][N:25]=2)=[CH:13][CH:14]=1)=[O:6].[OH-].[Mg+2:34].[OH-].[OH-].[Ca+2:37].[OH-]>C(O)(C)C.O>[CH3:1][CH2:2][CH2:3][CH2:4][C:5]([N:7]([C@H:26]([C:30]([OH:32])=[O:31])[CH:27]([CH3:29])[CH3:28])[CH2:8][C:9]1[CH:10]=[CH:11][C:12]([C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][C:20]=2[C:21]2[NH:22][N:23]=[N:24][N:25]=2)=[CH:13][CH:14]=1)=[O:6].[Ca:37].[Mg:34]

Participants

6

Reactant 3

HCID 73981Magnesium HydroxideHCID 6093208Calcium HydroxideHCID 178447302HCID 178447302, compound

Product 1

HCID 178447305HCID 178447305, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 3776IsopropanolSolvent

Procedure

21.5 g of valsartan in 200 ml of isopropanol and 100 ml of water are stirred for ca. 3 hours at ca. 25° C. with 1.5 g of magnesium hydroxide and 1.9 g of calcium hydroxide. The practically clear solution is concentrated in a vacuum at ca. 50° C. A total of 240 ml of ethyl acetate is added with stirring to the still warm, semi-solid residue which contains residual water. Upon stirring over night at ca. 25° C., initially sticky constituents are transformed into a homogeneous suspension. The suspension is filtered by suction and washed with 20 ml of ethyl acetate. The moist filter cake is dried in a vacuum at 30-40° C. A colourless crystal powder is obtained.

Workup

  1. concentrationThe practically clear solution is concentrated in a vacuum at ca. 50° C
  2. additionA total of 240 ml of ethyl acetate is added
  3. temperaturestill warm
  4. stirringUpon stirring over night at ca. 25° C.
  5. filtrationThe suspension is filtered by suction
  6. washwashed with 20 ml of ethyl acetate
  7. customThe moist filter cake is dried in a vacuum at 30-40° C
  8. customA colourless crystal powder is obtained

Sources & evidence

ORD record
ord-312362e432bf4ceb9fcd276d285a0cfc
Source dataset
uspto-grants-2012_10
Patent number
US08278339B2

Reaction notes

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