1,3-Propanediamine → HCID 15504442, compound

Temperature

130 °C

As shown in the following Reaction 9, 100 mg (0.42 mmol) of 2-(4-bromo-phenyl)-thiophene synthesized in C of Example 1-2 was melted in 5 mL of n-phentanol, and 130 mg (0.84 mmol, 2 eq) of sodium iodide and 0.004 mL (0.042 mmol, 10 mol %) of 1,3-diaminopropane was added thereto, and then the reaction solution was refluxed for 18 hours at temperature of 130° C. Next, the reaction solution was washed with aqueous ammonia, and was dehydrated with magnesium sulfate, filtered, and then distilled under reduced pressure. The compound distilled under reduced pressure was purified with a column chromatography (mobile phase: n-hexane) to obtain 100 mg of 2-(4-iodo-phenyl)-thiophene with the yield of 83.3%. NMR data of the obtained compound is as follows. [1H NMR (400 MHz, CDCl3): δ 7.52 (m, 4H), 7.33 (d, 2H), 7.10 (t, 1H)].

1. customsynthesized in C of Example 1-2
2. additionwas added
3. washNext, the reaction solution was washed with aqueous ammonia
4. filtrationfiltered
5. distillationdistilled under reduced pressure
6. distillationThe compound distilled under reduced pressure
7. customwas purified with a column chromatography (mobile phase: n-hexane)

ORD record

ord-0477247499c24f3796bc7dfb8158cb8a

Source dataset

uspto-grants-2010_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07850872B2