Lawesson's reagent → HCID 86671703, compound

Temperature

120 °C

In a 500 mL three-neck flask were put 18 g (74 mmol) of N-(4-bromophenyl)isobutyramide obtained in Step 1, 15 g (37 mmol) of 2,4-bis(4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane-2,4-disulfide (Lawesson's reagent), and 120 mL of toluene, and the mixture was heated and refluxed at 120° C. for 3 hours. After that, toluene was distilled off to give a yellow oily substance. This oily substance was purified by silica gel column chromatography. Toluene was used as a developing solvent. The resulting fraction was concentrated to give a yellow solid. The resulting solid was collected by suction filtration, and the collected solid was washed with a small amount of methanol to give 13 g of a white solid of N-(4-bromophenyl)isobutyrthioamide in a yield of 70%. The reaction scheme of Step 2 is shown in (b-2) below.

1. customIn a 500 mL three-neck flask were put
2. distillationAfter that, toluene was distilled off
3. customto give a yellow oily substance
4. customThis oily substance was purified by silica gel column chromatography
5. concentrationThe resulting fraction was concentrated
6. customto give a yellow solid
7. filtrationThe resulting solid was collected by suction filtration
8. washthe collected solid was washed with a small amount of methanol

ORD record

ord-348a614dcdb640ed94f75a22138f225e

Source dataset

uspto-grants-2015_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09155158B2