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13844289537
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note
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Experimental Procedure for Preparation of [(Dimethylphenylsilyl)methyl] Magnesium Chloride (1): Under an argon atmosphere, a suspension of magnesium turnings (0.14 g, 5.83 mmol) in refluxing THF (2 mL) was activated by addition of catalytic amounts of 1,2-dibromoethane. Then, (chloromethyl) dimethylphenylsilane (902.1 μL, 5 mmol) was added at such a rate as to maintain a gentle reflux. After the addition was complete, the solution became transparent and grayish. To this solution, additional THF was added to adjust the concentration to be 0.5 M or 1.0 M and the mixture was refluxed for 2 h to give THF solutions of 1. The concentration of THF solution of 1 was determined by the method of Orgura et al.23
-
-
-
-
50
-
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13844259616
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note
-
29NOSSi: 359.1739. Found: 359.1742.
-
-
-
-
51
-
-
13844294627
-
-
note
-
R(minor) = 16.15 min, (major) = 20.22 min.
-
-
-
-
52
-
-
13844278493
-
-
note
-
3): δ = 28.280, 57.079, 66, 688, 79.902, 126.525, 127.632, 128.686, 139.621, 156.016.
-
-
-
-
53
-
-
13844294629
-
-
note
-
R, R) in analogy with 3a.19 The absolute stereochemistry of 3a-f and amino alcohols 6a-f were determined by comparisons with known compounds.
-
-
-
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54
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0024787272
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Yamashita, H.2
Otsubo, T.3
Orgura, F.4
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