- Chiral spiro monophosphine-oxazoline ligands and preparation method thereof
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The invention provides chiral spiro monophosphine-oxazoline ligands as well as intermediates and a preparation method thereof. The ligands are structural compounds shown in the following formulas 1, 2and 3 and comprise racemates and optical isomers of the compounds, and m and n are integers of 0-3; X is CRR, NR, O or S; R1 and R2 are respectively and independently hydrogen, alkyl, phenyl, 1naphthyl, 2naphthyl, alkoxy and ester substituted alkyl; R is hydrogen, alkyl, substituted phenyl, substituted alkyl, alkoxy, phenyl, 1-naphthyl, 2-naphthyl, halogen, cyano, carboxyl and hydroxyl; R2 is hydrogen, alkyl, phenyl, 1-naphthyl, 2-naphthyl or alkyl substituted phenyl; M' is P(O)(R3)2 or P(R3)2; R3 is alkyl, phenyl, 1-naphthyl, 2-naphthyl, substituted phenyl, furyl or thienyl; M isOTf, COOH or COOR5; OTf is trifluoromethanesulfonic acid group; and R5 is alkyl.
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Paragraph 0293-0295
(2021/01/24)
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- Silodosin Intermediate and Preparation Method Therefor
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Disclosed are a silodosin intermediate and a preparation method thereof. The silodosin intermediate has the structure shown by the formula (A). X is hydrogen or bromide and R1 is hydrogen. The formyl group may be a group having the structure sh
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Paragraph 0109; 0110; 0111
(2015/06/03)
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- SILODOSIN INTERMEDIATE AND PREPARATION METHOD THEREFOR
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Disclosed are a silodosin intermediate and a preparation method thereof. The silodosin intermediate has the structure shown by the formula (A). X is hydrogen or bromide and R1 is hydrogen. The formyl group may be a group having the structure shown by the formula I. R7 is an carboxyl-protecting group, and R2 is 3-hydroxypropyl or a group having the structure shown by the formula II. W is a hydroxyl-protecting group. A compound of the formula (A) according to the present invention may further be used for preparing a compound having the structure shown by the formula (D). By means of the intermediate and the preparation method therefor provided by the present invention, high-purity optically pure silodosin can be obtained, and the optical purity is above 99%.
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Paragraph 0109; 0110
(2014/11/27)
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- First asymmetric synthesis of Silodosin through catalytic hydrogenation by using Ir-SIPHOX catalysts
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An asymmetric synthesis of Silodosin was accomplished in high yield via catalytic hydrogenation of α,β-unsaturated carboxylic acid derivatives by using chiral catalyst Ir-SIPHOX, followed by Curtius rearrangement. Copyright
- Yan, Pu-Cha,Zhang, Xian-Yi,Hu, Xiao-Wei,Zhang, Bin,Zhang, Xiang-Dong,Zhao, Michael,Che, Da-Qing,Li, Yuan-Qiang,Zhou, Qi-Lin
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supporting information
p. 1449 - 1451
(2013/04/10)
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