Sodium hydride → HCID 15434706, compound

HRID 1934864Notes

Reaction equation

HRID 1934864 reaction equation
[Br:1][C:2]1[C:3]([CH3:8])=[N:4][O:5][C:6]=1[NH2:7].[H-].[Na+].[C:11]1([P:17](Cl)([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[O:18])[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1>C1COCC1>[Br:1][C:2]1[C:3]([CH3:8])=[N:4][O:5][C:6]=1[NH:7][P:17]([C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1)([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)=[O:18]

Participants

5

Reactant 3

HCID 24758Sodium hydrideHCID 73910Diphenylphosphinic chlorideHCID 104875194-Bromo-3-methylisoxazol-5-amine

Product 1

HCID 15434706HCID 15434706, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

N-(4-bromo-3-methyl-5-isoxazolyl)diphenyl phosphinic amide was prepared by the method of Example 3 with 4-bromo-3-methyl-5-amino isoxazole (0.18 g, 1.0 mmol), THF (5 ml), NaH (60% oil dispersion, 88 mg, 2.2 mmol), and diphenyl phosphinic chloride (0.23 ml, 1.2 mmol). Recrystallization three times from chloroform and hexanes provided 0.17 g (45%) of faint pink crystals, m.p. 178.5-181° C.

Workup

  1. customRecrystallization three times from chloroform and hexanes

Sources & evidence

ORD record
ord-cdd2575290f7480887c369e63213e247
Source dataset
uspto-grants-2002_05
Patent number
US06384261B1

Reaction notes

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