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Page 1 of 17

1. Ç°ÑÔ

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2. õ£°·µÄÍÑË®·´Ó¦

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Page 2 of 17

2.1 ÓÃP2O5ΪÍÑË®¼ÁµÄ·´Ó¦ÊµÀý

OH2NP2O5OON

A solution of 35g (0.16 mol) of 2-(2-ethyl-3-benzofuranyl)-propionamide in 500ml of toluene was refuxed for 18 hours in the presence of P2O5. The organic phase was decanted off and the residue was carefully decomposed with ice-water and extracted with ether. The organic phase was washed with water, dried over sodium sulphate and added to the toluenic phase. The solvent was evaporated off under reduced pressure and the residue was fractionated to give 23.8g of 2-(2-ethyl-3-benzofuranyl)-propionitrile (yield 74.4%, boiling point: 105.deg. C. at0.2 mmHg).

Reference: US4124710 A1 (1978/11/07)

2.2 ÓÃPOCl3ΪÍÑË®¼ÁµÄ·´Ó¦ÊµÀý

OH2NSNNClPOCl3NSNNCl

A mixture of 2-chloro-1,3,4-thiadiazole-5-carboxamide (1.4 g) in 17 ml of POCl3 is heated at reflux for 18 hours. The reaction mixture is concentrated and the residue is suspended in 25 ml of ethyl acetate. The suspension is cooled in an ice bath and neutralized with saturated, aqueous NaHCO3 (to pH 7). The phases are separated and the aqueous phase is extracted with 20 ml of ethyl acetate. The combined organic phases are dried over MgSO4, filtered and concentrated. The residue is purified by column chromatography (using 30

percent

ethyl

acetate

/

hexane

as

eluent)

to

afford

0.832

g

of

2-cyano-5-chloro-1,3,4-thiadiazole. MP: 65-67. deg.C Reference: Patent; EP883611 B1 (2002/07/31)

2.3 ÓÃSOCl2ΪÍÑË®¼ÁµÄ·´Ó¦ÊµÀý

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