Methanol → HCID 178463218, compound

Participants

Reaction Steps

Add 21.8 L of methanol to 2.86 kg of biphenyl-4-carboxylic acid (R)-(6-(1-((4-fluorobenzyl)methylamino)ethylideneamino)-2(R)-hydroxyindan-1-yl)amide acetonitrile solvate. Pass the solution through a carbon impregnated filter and rinse the filter with 24 L of methanol. Add 5.7 kg of water to the solution over 35 min followed by 15 g of biphenyl-4-carboxylic acid (R)-(6-(1-((4-fluorobenzyl)methylamino)ethylideneamino)-2(R)-hydroxyindan-1-yl)amide hemihydrate seed crystals. After 20 min, add 1.15 kg of water followed by 15 g of seed crystals. After 1 h, add another 1.15 kg of water over 30 min followed by 15 g of seed crystals. After 10 min, add 3.4 kg of water over 1 h and stir the slurry at room temperature for 1 h and at 0° C. for 45 min. Collect the solid by filtration, rinse with a cold solution of 11.4 L of methanol and 2.9 L of water, and dry to afford 2.19 kg of the title compound as a white solid.

Provenance & Evidence