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15444369675
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note
-
The products 4, 5, 6, 9, 10, 11 (see Table 1) were obtained as an unseparable mixture of diastereoisomers using conventional chromatography.
-
-
-
-
45
-
-
15444371608
-
-
note
-
General Procedure for Radical Cyclization (4, 5, 6, 9, 10, 11). A solution of thiophenol (0.18 mL, 1.66 mmol) and AIBN (136 mg, 0.83 mmol) in benzene (16 mL) was added dropwise (8 mL/h) under an argon atmosphere to a boiling solution of 3 (200 mg, 0.83 mmol) in benzene (8 mL). The solvent was evaporated under reduced pressure. Purification of the residue by column chromatography (hexane-t-BuOMe, 20:1) afforded 9, 262 mg (90%, see Table 1).
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49
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15444370368
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note
-
1H NMR spectra were identical to those reported in the literature.
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52
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33748664603
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15444364480
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note
-
+: 313.1238; found: 313.1239.
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57
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0034625420
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58
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15444369489
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-
note
-
(b) 5% of sulfone was obtained.
-
-
-
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59
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0035844703
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60
-
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15444380118
-
-
note
-
+: 167.1072; found: 167.1070.
-
-
-
|