反应详情

温度

70 °C

The aqueous solution (280 ml.) of (+)-4,5,6,7-tetrahydro-7-oxobenzo[b]thiophen-4-amine hydrochloride from Example 53 is stirred while 40 grams of KOCN in 95 ml. of water is added dropwise. The mixture is warmed to 70° C. for 1.5 hour and cooled to 10° C. The light brown solid is collected and washed well with 700 ml. of water. The product is then stirred with 110 ml. of cold methanol, collected, and washed with 50 ml. of cold methanol to afford 48 grams of the title compound, m.p. 247°-249.5° C. (dec.), [α]D24 = - 97.16° (c, 0.14 in methanol).

1. temperaturecooled to 10° C
2. customThe light brown solid is collected
3. washwashed well with 700 ml
4. customof cold methanol, collected
5. washwashed with 50 ml