反应详情

5-Amino-2-(3(S)-(t-butoxycarbonyl)aminopyrrolidin-1-yl)fluorobenzene (30.4 g, 0.103 M) was dissolved in dry pyridine (150 ml) and cooled under nitrogen with stirring to 0°. Ethyl chloroformate (12.3, 0.113 M) was added dropwise, and the mixture stirred 1 hour at the same temperature. Ice-water (250 ml) was added, and stirring continued for 1 hour. The resulting precipitate was collected, washed thoroughly with water, and air dried. The residue was treated with toluene, azeotroped to half volume, then treated with isohexane (500 ml), to precipitate the desired product (35.3 g).

1. temperaturecooled under nitrogen
2. stirringthe mixture stirred 1 hour at the same temperature
3. stirringstirring
4. customThe resulting precipitate was collected
5. washwashed thoroughly with water, and air
6. customdried
7. additionThe residue was treated with toluene
8. customazeotroped to half volume
9. additiontreated with isohexane (500 ml)
10. customto precipitate the desired product (35.3 g)