関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetone | HCID 180 | — |
| 反応物 | 2-Acetylhydroquinone | HCID 10279 | — |
| 反応物 | Pyrrolidine | HCID 31268 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 6-Hydroxy-2,2-dimethylchroman-4-one | HCID 3519859 | 81.6% |
反応手順
A reaction mixture of 100 g (0.65 mol) of 2,5-dihydroxyacetophenone in 1 l of acetonitrile, 130 ml (1.55 mol) of pyrrolidine and 290 ml (3.95 mol) of acetone was heated at 45° C. for 8 h. The sol. were then removed i. vac. and the residue was dissolved in 1 l of EA. The organic phase was washed twice with dilute hydrochloric acid, stirred with activated carbon and dried over magnesium sulfate and substantially concentrated. The residue was stirred with petroleum ether and the precipitate was filtered off with suction giving 102 g of 2,2-dimethyl-6-hydroxychroman-4-one, m.p. 161° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06008245 |
|---|
| 出典データセット | uspto-grants-1999_12 |
|---|
| ORD ID | ord-ba9a7dbe4dde4653b6ac93c3127603d3 |
|---|
| 出典メモ | uspto-grants-1999_12 |
|---|