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Hydrochloric Acid → 7-Ethyl-9,10-dihydro-2-methyl-4H-benzo[5,6]cyclohepta[1,2-d]thiazol4-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Hydrogen Sulfide | HCID 402 | — |
| 反応物 | 7-Ethyl-9,10-dihydro-2-methyl-4H-benzo[5,6]cyclohepta[1,2-d]oxazol-4-one | HCID 22003584 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 7-Ethyl-9,10-dihydro-2-methyl-4H-benzo[5,6]cyclohepta[1,2-d]thiazol4-one | HCID 22003611 | — |
反応手順
A stirred suspension of potassium tert-butoxide (1.80 g) in dry N,N-dimethylformamide (20 ml) was cooled to 5° C. and saturated with hydrogen sulphide. The product from example 3 step (vi) (1.00 g) was added and the reaction stirred at room temperature for 1 hour. The mixture was poured into ice, acidified to pH4 with 2N hydrochloric acid and extracted with ethyl acetate. The extracts were washed with brine, dried (MgSO4) and evaporated to give an orange solid which was purified by chromatography eluting with 50% ethyl acetate in isohexane.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06218376B1 |
| 出典データセット | uspto-grants-2001_04 |
| ORD ID | ord-adbaab83bb094bc6ab27259c64182025 |
| 出典メモ | uspto-grants-2001_04 |