Id |
Subject |
Object |
Predicate |
Lexical cue |
T239 |
0-112 |
Sentence |
denotes |
Unless otherwise noted, materials were obtained from commercial suppliers and used without further purification. |
T240 |
113-266 |
Sentence |
denotes |
The removal of solvent under reduced pressure or concentration refers to distillation using a Büchi rotary evaporator attached to a vacuum pump (3 mmHg). |
T241 |
267-349 |
Sentence |
denotes |
Products obtained as solids or high-boiling oils were dried under vacuum (1 mmHg). |
T242 |
350-476 |
Sentence |
denotes |
Silica gel chromatography was performed on either a CombiFlash (Teledyne ISCO), SP4, or Isolera (Biotage) purification system. |
T243 |
477-677 |
Sentence |
denotes |
All reactions were performed under a positive pressure of nitrogen or argon or with a drying tube at an ambient temperature (unless otherwise stated) in anhydrous solvents, unless otherwise indicated. |
T244 |
678-847 |
Sentence |
denotes |
Analytical thin-layer chromatography (TLC) was performed on glass-backed silica gel 60 F254 plates (Analtech, 0.25 mm), eluting with the appropriate solvent ratio (v/v). |
T245 |
848-1018 |
Sentence |
denotes |
The reactions were assayed by high-performance liquid chromatography–mass spectrometry (LCMS) or TLC and terminated as judged by the consumption of the starting material. |
T246 |
1019-1189 |
Sentence |
denotes |
LCMS utilized wavelengths of 254 and 220 nm and either electrospray ionization (ESI) in positive mode or atmospheric-pressure chemical ionization (APCI) in positive mode. |
T247 |
1190-1294 |
Sentence |
denotes |
The TLC plates were visualized using UV light, p-anisaldehyde, phosphomolybdic acid, or iodine staining. |
T248 |
1295-1356 |
Sentence |
denotes |
Microwave-assisted reactions were run in a Biotage Initiator. |
T249 |
1357-1430 |
Sentence |
denotes |
1H NMR spectra were recorded on a Bruker XWIN-NMR (400 MHz) spectrometer. |
T250 |
1431-1527 |
Sentence |
denotes |
Proton chemical shifts are reported in parts per million downfield from tetramethylsilane (TMS). |
T251 |
1528-1618 |
Sentence |
denotes |
1H NMR data are reported as chemical shift (multiplicity, coupling constant, integration). |
T252 |
1619-1779 |
Sentence |
denotes |
Multiplicities are denoted as follows: s, singlet; d, doublet; t, triplet; q, quartet; dd, doublet of doublets; dt, doublet of triplets; and brs, broad singlet. |
T253 |
1780-1930 |
Sentence |
denotes |
For spectra obtained in CDCl3, DMSO-d6, and CD3OD, the residual protons (7.27, 2.50, and 3.31 ppm, respectively) were used as the internal references. |
T254 |
1931-2017 |
Sentence |
denotes |
The purity of the final products is >95% as determined by HPLC and/or 1H NMR analyses. |