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Water → 5-[[3,5-Bis(1,1-dimethylethyl)-4-hydroxyphenyl]methylene]-2-thioxo-4-imidazolidinone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 3,5-Di-tert-butyl-4-hydroxybenzaldehyde | HCID 73219 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | 2-Thiohydantoin | HCID 1274030 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 5-[[3,5-Bis(1,1-dimethylethyl)-4-hydroxyphenyl]methylene]-2-thioxo-4-imidazolidinone | HCID 54134253 | 57.8% |
反応手順
A mixture of 3,5-di-tert-butyl-4-hydroxybenzaldehyde (30.0 g, 128 mmols), 2-thiohydantoin (14.8 g, 128 mmols), and sodium acetate (36 g) in acetic acid (200 ml) is stirred under nitrogen and heated to reflux. After 24 hours the mixture is allowed to cool, and is stirred into water (2 L). After an hour the product is filtered off, washed three times with water, and dried. Recrystallization from acetonitrile gave the 5-[[3,5-bis(1,1-dimethylethyl)-4-hydroxyphenyl]methylene]-2-thioxo-4-imidazolidinone (24.6 g), mp 278°-279° C. (dec).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05290800 |
| 出典データセット | uspto-grants-1994_03 |
| ORD ID | ord-a59b2f68367049babe8d084d0602202c |
| 出典メモ | uspto-grants-1994_03 |