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Triphenylphosphine → tert-Butyl [3-(2,5-difluorophenoxy)propyl]carbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | Diisopropyl diazene-1,2-dicarboxylate | HCID 75555 | — |
| 反応物 | 2,5-Difluorophenol | HCID 94952 | — |
| 反応物 | tert-butyl N-(3-hydroxypropyl)carbamate | HCID 3838134 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | tert-Butyl [3-(2,5-difluorophenoxy)propyl]carbamate | HCID 86610028 | — |
反応手順
The solution of 2.50 g of 2,5-difluorophenol, 3-(Boc-amino)-1-propanol, 7.26 g of triphenylphosphine and tetrahydrofuran (30 ml) is cooled to 0° C. and admixed dropwise with 5.65 ml of diisopropyl azodicarboxylate. The reaction mixture is stirred at room temperature for a further 2 hours and subsequently concentrated by evaporation. The title compound is obtained as a yellowish solid from the residue by means of flash chromatography (SiO2 60F). Rf=0.34 (1:2 EtOAc-heptane); Rt=4.69.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07790715B2 |
| 出典データセット | uspto-grants-2010_09 |
| ORD ID | ord-27f21aeff56c45c69488690421f20d01 |
| 出典メモ | uspto-grants-2010_09 |