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Imidazole → 4-(tert-Butyldimethylsiloxy)phenol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Imidazole | HCID 795 | — |
| 反応物 | tert-Butyldimethylsilyl chloride | HCID 28928 | — |
| 反応物 | p-Hydroxyphenyl benzoate | HCID 75549 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-(tert-Butyldimethylsiloxy)phenol | HCID 597388 | — |
反応手順
4-Hydroxyphenyl benzoate (9.0 mmol) was dissolved in CH2Cl2 (9 mL/mmol), TBDMS-Cl (1.5 eq., 13.5 mmol) and imidazole (2.0 eq., 18.0 mmol) were added and the mixture was stirred at r.t. overnight. The mixture was diluted with MeOH (4.5 mL/mmol), and NaBH4 (2.5 eq., 22.5 mmol) was added slowly over 5 min (attention: vigorous gas evolution). The mixture was concentrated by removing CH2Cl2 under reduced pressure and the suspension was heated to 65° C. for 15 h.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08207174B2 |
| 出典データセット | uspto-grants-2012_06 |
| ORD ID | ord-76d530adac7142d98b992c5740c45a81 |
| 出典メモ | uspto-grants-2012_06 |