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ChemicalBook CAS DataBase List 2-METHYL-2-PENTANOL

2-METHYL-2-PENTANOL synthesis

11synthesis methods
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Yield:590-36-3 96.7%

Reaction Conditions:

Stage #1:1-propylmagnesium chloride;acetone in tetrahydrofuran at -5 - 0;
Stage #2: with water at 40;Reagent/catalyst;

Steps:

1
(1) into the reaction flask was added of 1-chloropropane Grignard reagent 240 ml with concentration of 1.83 mol / L, 21.23 g (0.37 mol) of acetone was weighed in a constant pressure dropping funnel, then 40 g of anhydrous THF was added and the mixture was homogeneously mixed. When the reaction flask internal temperature reached -5 ° C, began to drop the configured mixture of acetone and THF, control dropwise addition time between 0.5 ~ 1.0 hours, and the control reaction flask internal temperature to -5 ~ 0 °C. After completion of the dropwise addition, the reaction mixture incubated for 1 hour to obtain a condensation reaction solution. (2) into the the reaction flask was added 51.4 g of deionized water (2.86 mol). The condensation reaction solution obtained in step (1) was dropped into deionized water under a water bath. The dropping speed was controlled to ensure that the inside temperature of the reaction flask was not more than 40 ° C. inside the reaction flask gradually forms a loose solid magnesium salts. (3) After the hydrolysis reaction was completed, filtration was carried out, the filter cake was beaten and washed with 200 ml of anhydrous THF. The washing was finished , the mixture was dried and the filter cake was magnesium chloride and magnesium hydroxide crystalline complex. The filter cake was dried with THF to obtain 42 g of solid composite magnesium salt. Through XRD detection, the composition of the solid composite magnesium salt is Mg3(OH)4Cl2·4H2O), which can be sold directly or concentrated hydrochloric acid to prepare magnesium chloride sales. The water content of the filtrate is less than 1%. After the THF is recovered, obtained a 37.2 g of 2-methyl -2- pentanol , The content was 98.1%, the yield was 96.7%

References:

Zhejiang Xinhecheng Co., Ltd.;Zhang Qian;Wu Yuanyuan;Li Yuying;Shi Zheqin;Shi Zeyu;Wu Chaoyong;Shi Jin;Pan Zhujun;Wu Ying;Lv Yewen CN106699510, 2017, A Location in patent:Paragraph 0033-0037; 0051

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