One-pot synthesis of 6-bromo-4,4-dimethylthiochroman

Zhou, Shaodong; Liao, Zutai; Yuan, Ji-Xin; Qian, Chao; Chen, Xinzhi

doi:10.1007/s11164-012-0928-8

Cited by 1 publication

(1 citation statement)

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“…The typical synthetic scheme is shown in Figure 1. Detection and quantitation limits of the of 3,3-dimethylallyl bromide has to be demonstrated concerning the limit 10 ppm (toxicology limit as per the daily dosage of tazarotene), the 6-bromo-4,4-dimethylthiochroma was used in the synthesis of tazarotene drug substance, which was prepared from benzenethiol and 1-bromo-3-methylbut-2-ene [4]. Many analytical methods were available to quantify the tazarotene and its processed degradation impurities.…”

Section: Introductionmentioning

confidence: 99%

Quantitative method for determination of 3,3‐dimethylallyl bromide genotoxic impurity in Tazarotene drug substance by GC‐MS

Rajana

Ramana

Babu

et al. 2020

Separation Science Plus

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A highly sensitive gas chromatography‐mass spectrometry quantitative method was developed for 3,3‐dimethylallyl bromide genotoxic impurity in the tazarotene drug substance. The method was validated by following the International conference for harmonization Q2 (R1) guideline for the limit test of 3,3‐dimethylallyl bromide genotoxic impurity in the tazarotene drug substance. The 148 m/z, 150 m/z, and 69 m/z ions were selected to get a response in mass spectrometry for 3,3‐dimethylallyl bromide. DB‐1 (30 mm × 0.25 × 1.0 µm) column was used for the separation of 3,3‐dimethylallyl bromide from the sample matrix. The limit of detection and limit of quantitation for 3,3‐dimethylallyl bromide in this method was 0.7 and 2.1 ppm, respectively. The method was precise and accurate at limit of quantitation level, 1.7% RSD was observed at limit of quantitation precision and 100.9% recovery observed at limit of quantitation accuracy, it was linear from the 5 to 20 µg/L, the correlation coefficient (r) was 0.9996.

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Section: Introductionmentioning

confidence: 99%