反应详情

NaH (147 mg, 3.75 mmol) was washed with heptane, and suspended in THF (10 ml). N-(Tetrahydro-2H-pyran-2-yloxy) 2-[6-(naphthalene-2-sulfonylamino)-3-azabicyclo[3.1.0]hex-3-yl]pyrimidine-5-carboxamide (1.113 g, 2.2 mmol) was then added, followed by addition of dimethyl sulfate (0.22 ml, 2.3 mmol). The mixture was stirred for 48 h, then poured into DCM (150 ml). 2.4M ammonium chloride (50 ml) was added. The aqueous layer was further extracted with DCM (150 ml). The combined organic layers were dried (MgSO4) and concentrated in vacuo to give an orange oil. This was carried forward without any further purification.

1. extractionThe aqueous layer was further extracted with DCM (150 ml)
2. dry with materialThe combined organic layers were dried (MgSO4)
3. concentrationconcentrated in vacuo
4. customto give an orange oil
5. customThis was carried forward without any further purification