Methyl iodide → 4-Chloro-7-[3,5-bis-o-(2,4-dichlorophenylmethyl)-2-c,2-o-dimethyl-beta-d-ribofuranosyl]-7h-pyrrolo[2,3-d]pyrimidine

To a pre-cooled (0° C.) solution of the compound from Example 62, Step D (618 mg, 1.0 mmol) in THF (8 mL) was added methyl iodide (709 mg, 5.0 mmol) and NaH (60% in mineral oil) (44 mg, 1.1 mmol). The resulting mixture was stirred overnight at rt and then poured into a stirred mixture of saturated aqueous ammonium chloride (50 mL) and dichloromethane (50 mL). The organic layer was washed with water (50 m]L), dried (MgSO4) and evaporated in vacuo. The resulting crude product was purified on silica gel using ethyl acetate/hexane as the eluent. Fractions containing the product were pooled and evaporated in vacuo to give the desired product (735 mg) as a colorless foam.

1. washThe organic layer was washed with water (50 m]L),
2. dry with materialdried (MgSO4)
3. customevaporated in vacuo
4. customThe resulting crude product was purified on silica gel
5. additionFractions containing the product
6. customevaporated in vacuo

ORDレコード

ord-093417f270c4402ca304d715f9096374

出典データセット

uspto-grants-2006_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07125855B2