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Development of a Novel Process for the Kilogram-Scale Synthesis of Spiro[1H-pyrido[2,3-d][1,3]oxazine-4,4′-piperidine]-2-one
Organic Process Research & Development ( IF 3.1 ) Pub Date : 2018-07-26 00:00:00 , DOI: 10.1021/acs.oprd.8b00202 Dale R. Mowrey 1 , James J. Reif 1 , Karen L. Milkiewicz 1 , Shawn P. Allwein 1
Organic Process Research & Development ( IF 3.1 ) Pub Date : 2018-07-26 00:00:00 , DOI: 10.1021/acs.oprd.8b00202 Dale R. Mowrey 1 , James J. Reif 1 , Karen L. Milkiewicz 1 , Shawn P. Allwein 1
Affiliation
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Spiro[1H-pyrido[2,3-d][1,3]oxazine-4,4′-piperidine]-2-one (3) is a key building block in many biologically active compounds. The synthesis of this compound, as reported in the literature, is low-yielding. We have discovered and developed a robust, high-yielding process to generate 3 as a bis-HCl salt using alternative starting materials and reaction conditions. The developed process was successfully demonstrated on a kilogram scale. A two-batch kilo lab campaign generated the bis-HCl salt of 3 in >99 HPLC area percent purity and 77% overall yield.
中文翻译：
螺[1 H-吡啶[2,3- d ] [1,3]恶嗪-4,4'-哌啶] -2-one公斤级合成新工艺的开发
螺[1 H-吡啶并[2,3- d ] [1,3]恶嗪-4,4'-哌啶] -2-酮（3）是许多生物活性化合物的关键组成部分。如文献报道，该化合物的合成产率低。我们发现并开发了一种健壮的高产率工艺，可以使用替代的原料和反应条件生成3作为双HCl盐。所开发的过程已成功地以千克为单位进行了演示。两次批次的千斤实验室活动在＞ 99 HPLC面积百分比纯度中产生了3的双HCl盐，总产率为77％。
更新日期：2018-07-26
中文翻译：
螺[1 H-吡啶[2,3- d ] [1,3]恶嗪-4,4'-哌啶] -2-one公斤级合成新工艺的开发
螺[1 H-吡啶并[2,3- d ] [1,3]恶嗪-4,4'-哌啶] -2-酮（3）是许多生物活性化合物的关键组成部分。如文献报道，该化合物的合成产率低。我们发现并开发了一种健壮的高产率工艺，可以使用替代的原料和反应条件生成3作为双HCl盐。所开发的过程已成功地以千克为单位进行了演示。两次批次的千斤实验室活动在＞ 99 HPLC面积百分比纯度中产生了3的双HCl盐，总产率为77％。
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