Sulfuric acid magnesium salt (1:1) → HCID 59204391, compound

HRID 2241878Notes

Reaction equation

HRID 2241878 reaction equation
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[CH:11]([CH2:12][CH2:13][CH:14]([C:16]3[CH:21]=[CH:20][C:19]([F:22])=[CH:18][CH:17]=3)[OH:15])[C:10](=[O:23])[N:9]2[C:24]2[CH:33]=[CH:32][C:27]([C:28]([NH:30]O)=[NH:29])=[CH:26][CH:25]=2)=[CH:4][CH:3]=1.S([O-])([O-])(=O)=O.[Mg+2]>O1CCCC1.N.[Ni]>[F:1][C:2]1[CH:3]=[CH:4][C:5]([CH:8]2[CH:11]([CH2:12][CH2:13][CH:14]([C:16]3[CH:21]=[CH:20][C:19]([F:22])=[CH:18][CH:17]=3)[OH:15])[C:10](=[O:23])[N:9]2[C:24]2[CH:25]=[CH:26][C:27]([C:28]([NH2:30])=[NH:29])=[CH:32][CH:33]=2)=[CH:6][CH:7]=1

Participants

6

Reactant 2

HCID 24083Sulfuric acid magnesium salt (1:1)HCID 178513338HCID 178513338, compound

Product 1

HCID 59204391HCID 59204391, compound

Reagents, catalysts & solvents 3

HCID 935NickelCatalystHCID 222AmmoniaSolventHCID 8028TetrahydrofuranSolvent

Procedure

290 mg of 4-{2-(4-fluorophenyl)-3-[3-(4-fluorophenyl)-3-hydroxypropyl]-4-oxoazetidin-1-yl}-N-hydroxybenzamidine (12) were dissolved in 15 ml of tetrahydrofuran and, with 1.5 ml of conc. ammonia, hydrogenated over Raney nickel at 25° C. for 6.5 h. After addition of magnesium sulfate, the reaction solution was filtered. The filtrate was concentrated. This gave the product of molecular weight 435.48 (C25H23F2N3O2); MS (ESI): 436.18 (M+H+).

Workup

  1. filtrationthe reaction solution was filtered
  2. concentrationThe filtrate was concentrated
  3. customThis gave the product of molecular weight 435.48 (C25H23F2N3O2)

Sources & evidence

ORD record
ord-a6912961e925481a8e306e1f887ac9ce
Source dataset
uspto-grants-2010_03
Patent number
US07671047B2

Reaction notes

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