反应详情

100 mg (0.33 mmol) of unpurified 4-[(4-dipropylaminobutyl)methylamino]methylbenzonitrile (2b) synthesized in Example 5 was charged in a 25 ml recovery flask, and dissolved in 3 ml of methanol. After 290 mg (0.80 mmol, 2.4 equivalents) of a 10% hydrochloric acid-methanol solution was added dropwise to the solution under cooling with ice, the mixture was stirred for one hour. The reaction solution was then concentrated. After the addition of 5 ml of methanol to the residue, the mixture was reconcentrated. This operation was repeated twice, thereby obtaining 122 mg of 4-[(4-dipropylaminobutyl)methylamino]methylbenzonitrile hydrochloride (2ba) as a colorless oily substance (yield: 99%).

1. temperatureunder cooling with ice
2. concentrationThe reaction solution was then concentrated
3. additionAfter the addition of 5 ml of methanol to the residue