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ChemicalBook CAS DataBase List 4-CYANOCYCLOHEXANONE CYCLIC ETHYLENE ACETAL

4-CYANOCYCLOHEXANONE CYCLIC ETHYLENE ACETAL synthesis

4synthesis methods
-

Yield: 50%

Reaction Conditions:

with potassium tert-butylate in 1,2-dimethoxyethane at 0; for 2 h;

Steps:

116.1 Step 1
Step 1: t-BuOK (18.5 g, 165.2 mmol) was added into a solution of compound 116-1 (10 g, 64 mmol) and TosMIC(17.6 g, 90.27 mmol) in DME (10 mL) at 0 °C. The reaction mixture was stirred at 0°C for 2h. After the reaction wascomplete, the reaction mixture was quenched with saturated NH4Cl solution and extracted with EtOAc. The combinedextraction liquid was washed with brines, dried over sodium sulfate and concentrated to dry, finally purified by columnchromatography (PE:EtOAc = 1:1) to deliver 2 (6.7 g, yield 50%) as colorless oil.

References:

GUANGDONG ZHONGSHENG PHARMACEUTICAL CO., LTD;WU, Hao;LIN, Jun;LI, Yunhui;WEI, Changqing;CHEN, Shuhui;LONG, Chaofeng;CHEN, Xiaoxin;LIU, Zhuowei;CHEN, Lijuan EP3124482, 2017, A1 Location in patent:Paragraph 0211; 0212