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Trimethyl orthoformate → [3-(1,1-Dimethoxyethyl)-5-pentafluorosulfanylphenyl]dimethylamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trimethyl orthoformate | HCID 9005 | — |
| 反応物 | Orthoformate | HCID 21585117 | — |
| 反応物 | 1-(3-Dimethylamino-5-pentafluorosulfanylphenyl)ethanone | HCID 58085707 | — |
| 触媒 | D-Camphorsulfonic Acid | HCID 65617 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | [3-(1,1-Dimethoxyethyl)-5-pentafluorosulfanylphenyl]dimethylamine | HCID 58085701 | 96.9% |
反応手順
1-(3-Dimethylamino-5-pentafluorosulfanyl phenyl)ethanone (650 mg) was dissolved in methanol (50 ml) and treated with stirring with trimethyl orthoformate (715 mg) and DL-10-camphorsulfonic acid (10 mg). After stirring for 3 h, more orthoformate (200 mg) was added, and the mixture was stirred for 2 h and then allowed to stand overnight. The solvent was then stripped off and the residue was dried in a high vacuum. 730 mg of crude product were obtained, which were reacted directly in the next stage.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07863269B2 |
| 出典データセット | uspto-grants-2011_01 |
| ORD ID | ord-81c31f13f25a4b3e833e94d168e57d8f |
| 出典メモ | uspto-grants-2011_01 |