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Hexamethylenetetramine → 4-(2-Phenylpropan-2-yl)benzaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hexamethylenetetramine | HCID 4101 | — |
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | Dimethyldiphenylmethane | HCID 13065 | — |
| 生成物 | 4-(2-Phenylpropan-2-yl)benzaldehyde | HCID 18509413 | 80.5% |
反応手順
Trifluoroacetic acid (35 ml), was mixed with 3.93 g(20.0 mmol), of 2,2-diphenylpropane and 2.80 g (20.0 mmol), of hexamethylenetetramine and heated to reflux for 16 hours. After cooling to room temperature, the reaction mixture was poured into ice water and the mixture was stirred for 1 hour. The solution was adjusted to pH=about 9 and extracted with 100 ml of diethyl ether. The organic extract was washed with saturated saline and dried with sodium sulfate and the solvent was distilled off under reduced pressure. The resulting residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=10:1), to obtain 3.61 g (yield: 80.5%), of the target compound as a pale yellow oily substance.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06329399B1 |
| 出典データセット | uspto-grants-2001_12 |
| ORD ID | ord-27f16714ee9f40f4a690c202074ef496 |
| 出典メモ | uspto-grants-2001_12 |