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13
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-
84918622081
-
-
−3. A total of 928 reflections with 28 less than 116.0° were measured on an automated four-circle diffractometer using monochromatic copper radiation. The structure was solved using the direct methods routine SOLV of the SHELXTL program library (see Sheldrick, G. M. Shelxtl, Rev 4, Instrument Corporation, 1983) and was refined by the least squares method with anistropic temperature factors for all atoms except hydrogen. All hydrogen atoms, except the HBr salt hydrogen, were included with isotropic temperature factors at calculated positions. The final Rfactor was 0.059 for 817 unique observed reflections.
-
-
-
-
14
-
-
84918604148
-
-
Carbinolamine 9 has been referred to as “Darvon alcohol” at various points in the literature. This use of the Darvon® trademark has not been authorized by Eli Lilly and Company
-
-
-
-
15
-
-
0037673651
-
-
This material is sold by Aldrich Chem. Co. under the trademark Chirald ®. c, Industrially, 9 is obtained by classical resolution from the corresponding d,l mixture with (−)-camphorsulfonic acid in ethanol, Purified 8 is efficiently recovered from the mother liquors of 9 by resolution with the same acid in acetone. For this work 8 was obtained from Eli Lilly Industries, Mayaguez, Puerto Rico. See
-
(1955)
J. Am. Chem. Soc.
, vol.77
, pp. 3400
-
-
Pohland1
Sullivan2
-
16
-
-
0001130169
-
Design of chiral derivatizing agents for the chromatographic resolution of optical isomers. Asymmetric synthesis of some chiral fluoroalkylated amines
-
3, observe N-methyls - see, and by direct chiral HPLC assay on a Chiralcel® OD column using 0.2% [[Truncated]]
-
(1977)
The Journal of Organic Chemistry
, vol.14
, pp. 2436
-
-
Pirkle1
Hauske2
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19
-
-
84918622300
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-
Typically in a reduction employing 248 g of 8, the dried hexane layer is concentrated to 900 ml, cooled to −20 °C, and filtered. Concentration of the filtrate to 300 ml, re-cooling and filtration provides a second crop (total recovery = 84%).
-
-
-
-
20
-
-
84918609164
-
-
2 in toluene do not easily ignite.see Lithium Aluminium Hydride, 1987; Lithium Division of Chemetal. VHS-NTSC Video (englisch), Kinax Film- und Videoproduktion, Kopierwerk, Wilhelm Ax KG, Am Zwingel 6340 Dillenburg, Postfach 1542.
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-
-
-
21
-
-
84918632241
-
-
Because of the nature of the reagent, ee's fall to about 75% in 22-L equipment. However unpublished results of Louis Hibbard and Randy Hawley from this lab show that high ee's are maintained when the reaction is conducted through a 500 ml Zipperclaver reactor at < −70 °C.
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-
-
-
22
-
-
4243724631
-
-
Prepared in 86–91% yield (directly crystallized) by reaction of 2 with dimethylamine hydrochloride (0.83 Kg|Kg 2) and paraformaldehyde (0.36 Kg|Kg 2) using 12 N hydrochloric acid (16ml/Kg 2) in ethanol (2.45 L/Kg 2 reflux 20–24 h), Ital. Patent 637 371, 1962
-
(1964)
Chem. Abstr.
, vol.60
, pp. 479c
-
-
Plastino1
Loprieno2
Bugian3
Tenerini4
-
25
-
-
0023755363
-
-
The third entry of the Table was isolated in 94% yield and represents a candidate for the synthesis of R- or S-fluoxetine. For recent enantioselective syntheses of fluoxetine see
-
(1988)
J. Org. Chem.
, vol.53
, pp. 2916
-
-
Srebnik1
Ramachandran2
Brown3
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