Ethanol → 5-Thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid, 3-[[(5-methyl-1,3,4-thiadiazol-2-yl)thio]methyl]-8-oxo-7-[[2-(1H-tetrazol-1-yl)acetyl]amino]-, sodium salt, hydrate (1:1:5), (6R,7R)-

To a reactor equipped with a jacket were added 10 ml ethanol, 50 ml dichloromethane, 20 ml water, 5 g cefazolin acid and 0.9 g sodium acetate, stirred until the solution was clear, the finishing point pH was adjusted to be 7.4, the mixture was directly filtered into a glass crystallizer, agitated for 60 minutes, added dropwise about 20 ml of isopropanol and methanol mixed liquid (the amount of methanol is 3%) and methionine, turbidness occurred in the solution, hold for 4.0 hours, added isopropanol and methanol in a volume 10 times as much as the mixture at 1.5 MPa. The resultant was filtered, the filter cake was washed with acetic acid, dried at 80° C. for 0.5 hours to give cefazolin sodium pentahydrate.

1. customTo a reactor equipped with a jacket
2. filtrationthe mixture was directly filtered into a glass crystallizer
3. stirringagitated for 60 minutes
4. additionadded dropwise about 20 ml of isopropanol and methanol mixed liquid (the amount of methanol
5. additionadded isopropanol and methanol in a volume 10 times as much as the mixture at 1.5 MPa
6. filtrationThe resultant was filtered
7. washthe filter cake was washed with acetic acid
8. customdried at 80° C. for 0.5 hours

ORDレコード

ord-240e96b15b3f4e65a073bba9dac123d3

出典データセット

uspto-grants-2012_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08178521B2