Sodium Hydroxide → HCID 18381601, compound

HRID 2268893Notes

Reaction equation

HRID 2268893 reaction equation
C([O:3][C:4](=[O:28])[CH2:5][N:6]1[N:15]=[C:14]([CH2:16][C:17]2[C:22]([Cl:23])=[CH:21][N:20]=[CH:19][C:18]=2[Cl:24])[C:13]2[C:8](=[CH:9][C:10]([O:25][CH3:26])=[CH:11][CH:12]=2)[C:7]1=[O:27])C.[OH-].[Na+]>C(O)C>[Cl:24][C:18]1[CH:19]=[N:20][CH:21]=[C:22]([Cl:23])[C:17]=1[CH2:16][C:14]1[C:13]2[C:8](=[CH:9][C:10]([O:25][CH3:26])=[CH:11][CH:12]=2)[C:7](=[O:27])[N:6]([CH2:5][C:4]([OH:28])=[O:3])[N:15]=1

Participants

4

Reactant 2

HCID 14798Sodium HydroxideHCID 54477825HCID 54477825, compound

Product 1

HCID 18381601HCID 18381601, compoundYield 60%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A suspension of [4-(3,5-dichloro-pyridin-4-ylmethyl)-7-methoxy-1-oxo-1H-phthalazin-2-yl]-acetic acid ethyl ester (0.65 g, 1.54 mmoles), prepared as described in example 44, in ethanol (30 ml) was added with concentrated NaOH (3 ml). The mixture was stirred overnight at room temperature, then dried, taken up in water and washed twice with CH2Cl2. The aqueous phase was acidified with concentrated HCl. The precipitate was filtered and dried over P2O5 at 60° C., then crystallised from CH3OH (25 ml) and the filtrate was dried at 45° C. to give 0.36 g of the title compound (yield: 60%). m.p.: 221.4-222.4° C.

Workup

  1. customprepared
  2. customdried
  3. washwashed twice with CH2Cl2
  4. filtrationThe precipitate was filtered
  5. dry with materialdried over P2O5 at 60° C.
  6. customcrystallised from CH3OH (25 ml)
  7. customthe filtrate was dried at 45° C.

Sources & evidence

ORD record
ord-a06df8137cca4f55b0445ccc3ddef11b
Source dataset
uspto-grants-2001_12
Patent number
US06329370B1

Reaction notes

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