Hydrochloric Acid → O-(3-Methylisoxazol-5-yl)methylhydroxylamine hydrochloride

HRID 1451558Notes

Reaction equation

C(N)CCC.[CH3:6][C:7]1[CH:11]=[C:10]([CH2:12][O:13][N:14]2C(=O)C3=CC=CC=C3C2=O)[O:9][N:8]=1.[ClH:25]>C(O)C.C(OCC)C>[ClH:25].[CH3:6][C:7]1[CH:11]=[C:10]([CH2:12][O:13][NH2:14])[O:9][N:8]=1

Participants

Conditions

Temperature: 60 °C

Procedure

2.04 g of butylamine were added to a solution of 7.21 g of N-(3-methylisoxazol-5-yl)methoxyphthalimide [prepared as described in step (i) above] in 80 ml of ethanol, and the mixture was stirred for 1 hour at 60° C. At the end of this time, the temperature of the reaction mixture was lowered to room temperature, and then the reaction mixture was diluted with 300 ml of diethyl ether and acidified by the addition of a 10% by volume methanolic solution of hydrogen chloride at 0° C. The resulting crystals were collected by filtration, to afford 3.22 g of the title compound, melting at 193°-198° C.

Workup

customwas lowered to room temperature
filtrationThe resulting crystals were collected by filtration

Sources & evidence

ORD record: ord-91f37bafc9184d8eb5d7356dc41b0a21
Source dataset: uspto-grants-1997_02
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US05604256

Reaction notes

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