反应详情

MeOH (0.088 mL, 2.18 mmol) was added to a slurry of NaH (45 mg, 1.13 mmol) in DMF (2 mL). When gas evolution ceased, a solution of 3-bromo-5-(bromomethyl)benzonitrile (see WO2009/100169; 240 mg, 0.87 mmol) in DMF (1 mL) was added. The reaction was quenched by adding aq. sat NH4Cl solution. The mixture was partitioned between toluene (5 mL) and water (3 mL). The toluene layer was collected, washed with water, dried over Na2SO4, and concentrated in vacuo. The crude product was dried at reduced pressure and used in the next step: GCMS (CI) m/z 226 [M+H]+.

1. customThe reaction was quenched
2. additionby adding aq.
3. customThe mixture was partitioned between toluene (5 mL) and water (3 mL)
4. customThe toluene layer was collected
5. washwashed with water
6. dry with materialdried over Na2SO4
7. concentrationconcentrated in vacuo
8. dry with materialThe crude product was dried at reduced pressure