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Toluene → 5-[1-[3,5-Bis(1,1-dimethylethyl)-4-hydroxyphenyl]methylmethylene]-3-(dimethylamino)-2-thioxo-4-thiazolidinone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Ammonium Acetate | HCID 517165 | — |
| 反応物 | 3',5'-Bis(tert-butyl)-4'-hydroxyacetophenone | HCID 616296 | — |
| 反応物 | 4(5H)-Thiazolone, 3-(dimethylamino)dihydro-2-thioxo- | HCID 4341978 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 5-[1-[3,5-Bis(1,1-dimethylethyl)-4-hydroxyphenyl]methylmethylene]-3-(dimethylamino)-2-thioxo-4-thiazolidinone | HCID 57113872 | — |
反応手順
To 675 ml of toluene were added 20.9 g of 1-[3,5-bis(1,1-dimethylethyl)-4-hydroxyphenyl]ethanone, 13.3 g of N-dimethylaminorhodanine 6.5 g of ammonium acetate and about 20 ml of acetic acid. The mixture was heated at reflux temperature and any aqueous layer generated was collected in a Dean-Stark trap. Over the following 52 hours an additional 39 g of ammonium acetate and about 100 ml of acetic acid were added in increments and a total of 89.2 ml of aqueous phase was drawn off. Following workup by conventional techniques, 17.1 g of the desired subtitled intermediate was recovered.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05731336 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-c1a0b94f8eae41118a0fa90768e7a49a |
| 出典メモ | uspto-grants-1998_03 |