Synthesis of isotopically labelled 2‐isopropylthioxanthone from 2,2′‐dithiosalicylic acid and deuterium cumene

Abstract

Two efficient synthetic routes of stable deuterium labelled 2-isopropylthioxanthone were presented with 98.1% and 98.8% isotopic abundance in acceptable yields and excellent chemical purities. Their structures and the isotope-abundance were confirmed according to proton nuclear magnetic resonance and liquid chromatography-mass spectrometry.

Efficient synthesis of D6‐clenproperol and D6‐cimaterol using deuterium isopropylamine as labelled precursor

“…Based on the previous work about the synthesis of (1,3‐D 6 )‐2‐bromopropane before, the strategy of labelling deuterium on isopropyl group was designed. The 5‐step synthesis of the labelled isopropylamine 6 started with commercially available D 6 ‐acetone as depicted in Scheme . First of all, D 6 ‐acetone 1 was reduced with the minimum amount of LiAlH 4 to (1,3‐D 6 )‐propan‐2‐ol 2 with 99.8% atom D at 0°C (93.6% yield).…”

A Convenient Synthesis of β,β-Difluoro-β-iodo-1-phenylethan-1-ols

“…前期我们课题 组设计并合成了一系列的含 α,α,α-二氟碘代酮类化合物, 并将其用于各类二氟甲基化反应 [10] [11] 时, 也能以较好的收 率得到产物 2a, 也伴随着少量的羰基与碘同时被还原 的 产 物 4a 生 成 (Entry 2). 当 尝 试 还 原 能 力 较 强 的 LiAlH 4 [12] 时(Entry 3)发现, 得到的产物较为复杂, 通过 GC 检测到有 2a, 3a, 4a 三种不同的还原产物. 可见 LiAlH 4 作为还原剂对 α,α,α-二氟碘苯乙酮的还原选择性 较差, 反应效果不好.…”