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Acetic acid, (phenylthio)-, ethyl ester → 6-Ethyl 1-tert-butyl 2-dimethylamino-5-phenylthio-2,4-hexadienedioate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic acid, (phenylthio)-, ethyl ester | HCID 97312 | — |
| 反応物 | Diethyl 2-dimethylamino-5-phenylthio-2,4-hexadienedioate | HCID 86743580 | — |
| 反応物 | N(3-dimethylamino-3-t-butyloxycarbonylpropenylidene)-N-methylmethanaminium tetrafluoroborate | HCID 131716212 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | 6-Ethyl 1-tert-butyl 2-dimethylamino-5-phenylthio-2,4-hexadienedioate | HCID 131716211 | — |
反応手順
The procedure is as in Example 2 for the preparation of diethyl 2-dimethylamino-5-phenylthio-2,4-hexadienedioate, starting with N(3-dimethylamino-3-t-butyloxycarbonylpropenylidene)-N-methylmethanaminium tetrafluoroborate (4.05 g), a 1.6M solution (8.8 cc) of butyllithium in hexane and ethyl (phenylthio)acetate (2.8 g) in tetrahydrofuran (65 cc). After purification by chromatography on a silica column with a mixture of cyclohexane and ethyl acetate (70:30 by volume) as eluent, 6-ethyl 1-tert-butyl 2-dimethylamino-5-phenylthio-2,4-hexadienedioate (2.6 g), m.p. 85°-88° C., is obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04886835 |
| 出典データセット | uspto-grants-1989_12 |
| ORD ID | ord-c8c762a8393540459b15feb7cd32495a |
| 出典メモ | uspto-grants-1989_12 |