Hydrochloric Acid → 3-(3-Aminopropyl)benzamide

A mixture of 15.42 g (0.05 mole) N-[3-(3-carbamoylphenyl)propyl]phthalimide (the product of step (e)), 2.76 g (0.055 mole) hydrazine monohydrate and 100 ml ethanol was refluxed for about four hours under argon with heat, and then allowed to stir overnight. The reaction mixture was acidified with 30% (v/v) hydrochloric acid to a pH of about 1. Additional ethanol (about 10 to 20 ml) was added to the thick mixture. The mixture was filtered; the solids were rinsed with ethanol. The filtrate was evaporated to give a solid. Water (about 15 ml) was added to the solid; the resulting mixture was filtered. The filtrate wa basified with dry potassium carbonate until saturated, then extracted three times with 20 ml butanol. The butanol extracts were dried over sodium sulfate and potassium carbonate overnight, filtered and stripped to give 4.25 g of the above-identified product.

1. temperaturewas refluxed for about four hours under argon
2. temperaturewith heat
3. filtrationThe mixture was filtered
4. washthe solids were rinsed with ethanol
5. customThe filtrate was evaporated
6. customto give a solid
7. filtrationthe resulting mixture was filtered
8. extractionthen extracted three times with 20 ml butanol
9. dry with materialThe butanol extracts were dried over sodium sulfate and potassium carbonate overnight
10. filtrationfiltered

ORDレコード

ord-70a006006f77445b8dc480960ec19ed3

出典データセット

uspto-grants-1994_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05286252