Table 2. Screening of the Mitsunobu Reaction on a 50 g Scale (Scheme 2).
| entry | solvent | volume (mL) | temperature (°C) | TPPO-H2DIAD (dry) by filtration (g) | product isolation | yield (%) |
|---|---|---|---|---|---|---|
| 1 | THF | 250 | 0–5 | 0 | column | 71 |
| 2 | toluene | 500 | 25–30 | 0 | column | 70 |
| 3 | toluene | 500 | –5–0 | 5.5 | column | 70 |
| 4 | toluene | 200 | 25–30 | 10 | column | 70 |
| 5 | toluene | 200 | –5–0 | 75 | IPA (125 mL) | 68 |