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简单的萃取也可以发个Org. Process Res. Dev. 评论,亚氢钠如何有效除醛?

来源:行情   2024年12月13日 12:18

验了一下,位点仅限于,发掘造出此原理官能团耐受度极高,位点应用仅限于密切相关,但由于亚氢钠是含水的,对于脂质仲胺的分离缺点不佳。

另外一些高活性的内酯,也可以通过此原理转化成。

醇和逐步形成 亚氢钠烯醇可作是一个催化反应的基本概念,把普遍存在于基本概念中所微幅度的亚氢钠用酸或硫随之地转化成,其结果是烯醇可作又分解成取而代之的醇和,因此也可以通过此原理投放醇和或分离醇和。

标准化操作

Standard work-up procedure for aldehyde and ketone removal.

Substrate (1.4 mmol) and aldehyde (1.4 mmol) were dissolved in 5 mL MeOH, 25 mL saturated NaHSO3(aq) added, shaken for approximately 30 s, diluted with 25 mL H2O, and extracted with 25 mL 10% EA/hexanes. The organic layer was dried (MgSO4), filtered, and concentrated in vacuo to yield the recovered substrate.

Work-up procedure for non-polar aldehyde and ketone removal.

Substrate (1.4 mmol) and aldehyde (1.4 mmol) were dissolved in 10 mL DMF, 25 mL saturated NaHSO3(aq) added, shaken for approximately 30 s, diluted with 25 mL H2O, and extracted with 25 mL 10% EA/hexanes. The aqueous layer was extracted with 25 mL of 10% EA/hexanes. The combined organic layers were washed three times with H2O (25 mL, 10 mL, 5 mL). The organic layer was dried (MgSO4), filtered, and concentrated in vacuo to yield the recovered substrate.

Work-up procedure for isolation of both aldehyde and ketone.

Benzyl butyrate (250 μL, 1.4 mmol) and aldehyde 20 (275.0 mg, 1.4 mmol) were dissolved in 10 mL DMF, 25 mL saturated NaHSO3(aq) added, shaken for approximately 30 s, diluted with 25 mL H2O, and extracted with 25 mL 10% EA/hexanes. The aqueous layer was extracted with 25 mL of 10% EA/hexanes three times. The organic layers were washed three times with H2O (25 mL, 10 mL, 5 mL). The organic layer was dried (MgSO4), filtered, and concentrated in vacuo to yield recovered benzyl butyrate (261.3 mg, 98% recovery). The combined aqueous layers were basified with 50% sodium hydroxide and extracted with 25 mL of 10% EA/hexanes three times. The organic layers were washed three times with H2O (25 mL, 10 mL, 5 mL). The organic layer was dried (MgSO4), filtered, and concentrated in vacuo to yield recovered aldehyde 20 (261.3 mg, 95% recovery).

简介

Liquid–Liquid Extraction Protocol for the Removal of Aldehydes and Highly Reactive Ketones from Mixtures, Org. Process Res. Dev. 2017, 21, 9, 1394–1403

题外话,这个化学反应既然这么短时间,是不是可以用以除室内甲醇和?

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