関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Isopropylamine | HCID 6363 | — |
| 反応物 | Phenyl Isothiocyanate | HCID 7673 | — |
| 反応物 | Methyl bromoacetate | HCID 60984 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | HCID 178457009 | HCID 178457009 | — |
反応手順
To a solution of isopropylamine (1.31 g, 22.19 mmol) in methanol (25 mL) is added portionwise phenylisothiocyanate (3.0 g, 22.19 mmol). The solution which becomes slightly warm during the addition is stirred at rt for 4 h before pyridine (2.63 g, 33.29 mmol) and methyl bromoacetate (3.39 g, 22.19 mmol) is added. The mixture is stirred for another 16 h at rt before it is poured onto 1 N aq. HCl (100 mL) and extracted with diethyl ether (150 mL). The aq. layer is neutralised by adding sat. aq. NaHCO3 and extracted with diethyl ether (4×150 mL). The organic extracts are dried over MgSO4 and evaporated. The remaining solid is suspended in diethyl ether/heptane, filtered off, washed with additional diethyl ether/heptane and dried to give 3-phenyl-2-[(Z)-isopropylimino]-thiazolidin-4-one.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08524752B2 |
|---|
| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-4eb34ee1f82545c0b033ad06916456d0 |
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| 出典メモ | uspto-grants-2013_09 |
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