反应详情

875 Mg. 3-cyano-8-nitrodibenzo[b,f]thiepin-5,5-dioxide are dissolved in 105 cc. tetrahydrofuran. 15 CC. concentrated hydrochloric acid is added, followed by 3.8 g. stannous chloride dihydrate and the mixture is stirred for 24 hours. A solution of 20% sodium hydroxide is added, the mixture is shaken and the organic layer separated; the aqueous phase extracted once with ethyl acetate. The combined organic extracts are dried over sodium sulfate and evaporated to dryness. The residue is chromatographed on silica gel to yield 464 mg. (58%) pure amino compound, m.p. 321°-324° C.

1. customthe organic layer separated
2. extractionthe aqueous phase extracted once with ethyl acetate
3. dry with materialThe combined organic extracts are dried over sodium sulfate
4. customevaporated to dryness
5. customThe residue is chromatographed on silica gel
6. customto yield 464 mg