化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → 3,5,6,7-Tetrahydro-2-methyl-s-indacen-1(2H)-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Indane | HCID 10326 | — |
| 反応物 | Methacryloyl chloride | HCID 13528 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3,5,6,7-Tetrahydro-2-methyl-s-indacen-1(2H)-one | HCID 10954259 | — |
反応手順
Methacryloyl chloride (50 ml, 0.5 mol) was added to suspension of 133.5 r AlCl3 (1 mol) in 500 ml CH2Cl2 at −78° C., stirred 20 min. Then indane (59 g, 0.5 mol) was added at the same temperature, allowed to warm to room temperature and then was stirred overnight. Next day the mixture obtained was poured carefully into mixture of ice (1000 g) and HCl (200 ml). The organic phase was separated, washed by water, 5% NaHCO3, and dried over MgSO4. Solvent was evaporated and residue was distilled in vacuum given 77.6 of product (83%), b.p. 118-120° C./0.5 torr.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08207269B2 |
| 出典データセット | uspto-grants-2012_06 |
| ORD ID | ord-75ec45925fb84254861ee6335275f203 |
| 出典メモ | uspto-grants-2012_06 |