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Instruction of (3R,3aS,4S,4aS,7R,9aR)-1,3,3a,4,4a,5,6,7,8,9a-Decahydro-3-methyl-7-nitro-1-oxo-N,N-diphenylnaphtho[2,3-c]furan-4-carboxamide: A Comprehensive Guide for Chemical Engineers
Introduction:
(3R,3aS,4S,4aS,7R,9aR)-1,3,3a,4,4a,5,6,7,8,9a-Decahydro-3-methyl-7-nitro-1-oxo-N,N-diphenylnaphtho[2,3-c]furan-4-carboxamide is a complex compound used in various chemical reactions.
It is an important intermediate in the synthesis of several pharmaceuticals, agrochemicals, and other products.
The preparation of this compound involves several steps, and the process can be optimized for maximum yield and purity.
This article provides a detailed instruction for the synthesis of (3R,3aS,4S,4aS,7R,9aR)-1,3,3a,4,4a,5,6,7,8,9a-Decahydro-3-methyl-7-nitro-1-oxo-N,N-diphenylnaphtho[2,3-c]furan-4-carboxamide.
Materials:
The following materials are required for the synthesis of (3R,3aS,4S,4aS,7R,9aR)-1,3,3a,4,4a,5,6,7,8,9a-Decahydro-3-methyl-7-nitro-1-oxo-N,N-diphenylnaphtho[2,3-c]furan-4-carboxamide:
- 3-Methyl-7-nitro-2H-1,2,3-triazolo[1,2-d]benzoxazepine (Intermediate A)
- Sodium hydroxide (NaOH)
- N-Isobutyl iodide
- Diphenylphosphoryl azide (DPPA)
- Pyridine
- Hydrochloric acid (HCl)
- Methanol
- Water
- 1-Bromo-3-methyl-7-nitro-2H-1,2,3-triazolo[1,2-d]benzoxazepine (Intermediate B)
Equipment:
The following equipment is required for the synthesis of (3R,3aS,4S,4aS,7R,9aR)-1,3,3a,4,4a,5,6,7,8,9a-Decahydro-3-methyl-7-nitro-1-oxo-N,N-diphenylnaphtho[2,3-c]furan-4-carboxamide:
- 500-mL round-bottomed flask
- Magnetic stirrer
- Reflux condenser
- Glass stirring rod
- Thermometer
- Heat source
- Filter paper
- Buchner funnel
- Rotary evaporator
- Melting point apparatus
- HPLC system
Procedure:
Step 1: Preparation of Intermediate A
To a solution of 2-methyl-7-nitro-1,3-benzoxazepine (1 equiv) in carbon tetrachloride (100 mL), sodium