反应详情

温度

-10 °C

Triethylamine (444 mg., 4.4 mmole) is added to a suspension of 6-amino-2,2-dimethyl-3-cyanopenam (468 mg., 2 mmole) in methylene chloride (20 ml.) and the resulting mixture cooled to -10° C. A solution of α,α-di(2-methylphenyl)benzyl chloride (614 mg., 2 mmole) in methylene chloride (12 ml.) is added over a ten minute period and the resulting yellow solution stirred for one hour at -10° C. The cooling bath is removed and the mixture stirred and allowed to warm to room temperature. It is stirred for two hours at room temperature and is then concentrated under reduced pressure to a brown sludge. The sludge is chromatographed on a silica gel column (70-23- mesh., 380 × 20 mm. column) using chloroform as eluent. Fractions (15 ml. each) are collected. Fractions 13-19 are combined and concentrated in vacuo to dryness to give 155 mg. of product as a foam.

1. customThe cooling bath is removed
2. stirringthe mixture stirred
3. temperatureto warm to room temperature
4. stirringIt is stirred for two hours at room temperature
5. concentrationis then concentrated under reduced pressure to a brown sludge
6. customThe sludge is chromatographed on a silica gel column (70-23- mesh., 380 × 20 mm. column)
7. customeach) are collected
8. concentrationconcentrated in vacuo to dryness
9. customto give 155 mg