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Pyridine → Ammonia dichloromethane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | tert-Butyldimethylsilyl chloride | HCID 28928 | — |
| 反応物 | HCID 178418316 | HCID 178418316 | — |
| 反応物 | HCID 178418337 | HCID 178418337 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | Ammonia dichloromethane | HCID 22731429 | — |
| 生成物 | HCID 178418337 | HCID 178418337 | — |
反応手順
TBDMS protected histidinol 14--To a stirred solution of 205 mg (5.1 mmol) of NaH washed 3× with hexane, under argon, in 3.0 mL DMF was added in portions 500 mg (2.3 mmol) of histidinol dihydrochloride, resulting in moderate gas evolution. The solution was stirred for 1.5 h, then 1.8 mL (23 mmol) of anhydrous pyridine and 693.0 mg (4.6 mmol) of TBDMSCl was added. The solution was stirred for 1.5 h, concentrated in vacuo and flash chromatographed on silica with 15% CH3OH.NH3 /CH2Cl2 to yield 14.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05723592 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-48ed68423d4a4e7fb6e576167938191c |
| 出典メモ | uspto-grants-1998_03 |