1-Chloroethyl cyclohexyl carbonate synthesis
- Product Name:1-Chloroethyl cyclohexyl carbonate
- CAS Number:99464-83-2
- Molecular formula:C9H15ClO3
- Molecular Weight:206.67
50893-53-3
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99464-83-2
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Yield:99464-83-2 94%
Reaction Conditions:
with pyridine in dichloromethane at 0 - 20;
Steps:
4
EXAMPLE 4 Synthesis of PGB-03 (3-Aminomethyl-5-methyl-hexanoic acid 1-cyclohexyloxycarbonyloxy-ethyl ester) Procedure: Cyclohexy alcohol (1.4 g, 13.97 mmol) was dissolved in CH2Cl2 (15 mL) under the treatment in a nitrogen atmosphere (0-5° C.). 1-Chloroethyl chloroformate (2.0 g, 13.97 mmol) and CH2Cl2 (10 mL) were slowly added. The solution was stirred for 15 minutes and pyridine (1.22 g, 15.42 mmol) and CH2Cl2(2 mL) were added dropwise. After stirring overnight at room temperature, CH2Cl2 (20 mL) and water (20 mL) were added to the reaction solution. The product was extracted to the CH2Cl2 phase and washed with water (3*20 mL). The residue was dried and concentrated to give 2.64 g of Carbonic acid cyclohexyl ester 1-chloro-ethyl ester 6 (Yield: 94%). 1H-NMR (CDCl3, 500 MHz) δ 1.22-1.30 (m, 1H), 1.32-1.41 (m, 2H), 1.42-1.58 (m, 3H), 1.71-1.80 (m, 2H), 1.83 (d, J=6.0 Hz, 3H), 1.89-2.00 (m, 2H), 4.65-4.72 (m, 1H), 6.43 (q, J=6.0 Hz, 1H).
References:
Hwang, Jenn-Tsang;Hwang, Chrong-Shiong;Chang, Yow-Lone;Yao, Chung-Niang US2008/125483, 2008, A1 Location in patent:Page/Page column 6-7
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99464-83-2
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