反应详情

[(3S)-6-({2′,6′-Dimethyl-4′-[3-(methylsulfonyl)propoxy]biphenyl-3-yl}methoxy)-2,3-dihydro-1-benzofuran-3-yl]acetic acid (212.60 g) was dissolved in acetone (510 mL). Water (255 mL) was added dropwise. Seed crystal was added, and the mixture was stirred for 2 hr. The mixture was cooled to 10° C. or below, and stirred for 2 hr. While cooling to 10° C. or below, water (765 mL) was added dropwise, and the mixture was stirred for 2 hr. The precipitated solid was collected by filtration, and washed with a mixed solution (1360 mL) of acetone.water (1:4). The obtained solid was dried at 50° C. under reduced pressure to give [(3S)-6-({2′,6′-dimethyl-4′-[3-(methylsulfonyl)propoxy]biphenyl-3-yl}methoxy)-2,3-dihydro-1-benzofuran-3-yl]acetic acid hydrate as crystals (190.94 g). 100% ee.

1. additionSeed crystal was added
2. temperatureThe mixture was cooled to 10° C. or below
3. stirringstirred for 2 hr
4. temperatureWhile cooling to 10° C. or below
5. stirringthe mixture was stirred for 2 hr
6. filtrationThe precipitated solid was collected by filtration
7. washwashed with a mixed solution (1360 mL) of acetone
8. customThe obtained solid was dried at 50° C. under reduced pressure