D-Tryptophan methyl ester hydrochloride differential

D-Tryptophan methyl ester hydrochloride as fair apparent solid with its melting point 213-216° C ( lit. ) .The melting point is C.Its abstention is not beneath 205°than 98% ( N ) .The blueprint is 5G or 25G.This artefact should be stored amid 2-8° C. yield 0.30g of the product, additional 1mol/L hydrochloric acerbic band-aid of 1ml, additional bulk of dissolved, and adulterated to 20ml, as for the sample solution; attention admeasurement able quantity, baptize into the 1ml anniversary absolute 75 μ g solution, as a ascendancy solution. Thin band chromatography adjustment ( Appendix V B ) test, to draw the two kinds of band-aid of the 2 μ L, respectively, in the aforementioned silica gel G thin-layer plate, n-butyl booze and acerb acerbic / baptize ( 3:1:1 ) as developing solvent, afterwards expansion, drying, aerosol to indinavir three ketone with acetone ( 1 →50 ), at 80 ℃ for 10 account to dry, the actual appearance for the sample solution, the birthmark atom blush and adverse band-aid in the capital spot, shall not be added ( 0.5%).

D-Tryptophan methyl ester hydrochloride, at 105℃dry 3 hours, bargain weight accident shall not beat 0.2% alertness : yield no ice acerb acerbic (according to the baptize agreeable calculation, anniversary 1g baptize and acerb anhydride 5.22mL ) 750mL, abacus perchloric acerbic ( 70~72% ) 8.5mL, shaken, let cool, add adapted bulk of anhydrous acerb acerbic into 1000mL, strain, placed for 24 hours. If the abstinent sample calmly acetylation, have to use damp assurance adjustment for the assurance of the aqueous baptize content, and again baptize and acerb anhydride is adapted to the aqueous baptize agreeable of 0.01%~0.2%. Calibration: at 105 ℃drying to connected weight baseline adjoining benzene two formic acerbic hydrogen potassium about 0.16g, accurately weighed, and anhydrous acerb acerbic 20mL dissolved, add 1 drops of clear violet indicator liquid, the aqueous boring titrated to blue, and the titration after-effects application bare correction. Anniversary 1mL perchloric acerbic titration band-aid ( 0.1mol/L ) is agnate to the 20.42mg of the adjoining benzene two formic acerbic hydrogen potassium. According to the aqueous burning and adjoining benzene two formic acerbic hydrogen potassium and dosage, affected the aqueous concentration.

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From: chemical materials