Diiodomethane → HCID 15341799, compound

Temperature

0 °C

The compound of Example 5 (1.0 g, 4.8 mMol) was dissolved in methylene chloride (20 cm3) and transferred to a 100 ml three-neck round bottom flask under an argon atmosphere at 0° C. Triisobutylaluminum (2.95 g, 3.76 ml, 14.9 mmol) was added dropwise via a dropping funnel. The reaction mixture was stirred for about 20 minutes while maintaining the temperature at 0° C., then methylene iodide (1.67 g, 0.5 ml, 6.2 mmol) was added via syringe, and the reaction mixture was stirred at room temperature for about four hours then slowly poured into an ice cold solution of 10% sodium hydroxide. The aqueous layer was extracted twice with about 25 ml of methylene chloride, and all of the organic fractions were combined, dried over magnesium sulfate and concentrated in vacuo to give the product.

1. customtransferred to a 100 ml three-neck round bottom flask under an argon atmosphere at 0° C
2. stirringthe reaction mixture was stirred at room temperature for about four hours
3. extractionThe aqueous layer was extracted twice with about 25 ml of methylene chloride
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated in vacuo
6. customto give the product

ORD record

ord-093abc86114a47c49a63a2cd70c91e6f

Source dataset

uspto-grants-1995_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05439937