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HRID875921

反应详情

EQUATION

反应方程式

HRID 875921 的结构方程式

REACTANTS

反应物

2
结构：CC(C)(C)OC(=O)N[C@@H]1CCCNC1
HCID1514172

(R)-3-Boc-aminopiperidine

C10H20N2O2

结构：O=C(Nc1c[nH]c2ncc(Br)c(F)c12)[C@@H]1C[C@H]1c1ccccc1
HCID67045175

未命名化合物

PRODUCTS

生成物

1
结构：CC(C)(C)OC(=O)N[C@@H]1CCCN(c2c(Br)cnc3[nH]cc(NC(=O)[C@@H]4C[C@H]4c4ccccc4)c23)C1
HCID86652144

未命名化合物

收率 48.5%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CCC(C)O
溶剂HCID6568

2-Butanol

C4H10O

PROCEDURE

实验过程

trans-N-(5-Bromo-4-fluoro-1H-pyrrolo[2,3-b]pyridin-3-yl)-2-phenylcyclopropanecarboxamide (500 mg, 1.34 mmol) and (R)-tert-butyl piperidin-3-ylcarbamate (1338 mg, 6.68 mmol) in s-BuOH (5 mL) were heated to 135° C. in a sealed tube for 24 hours. After cooling down, the residue was concentrated and purified by reverse phase chromatography (SP4, 25M, water/ACN 80/20→0/100, 30 CV) to yield tert-butyl (R)-1-(5-bromo-3-(trans-2-phenyl cyclopropanecarboxamido)-1H-pyrrolo[2,3-b]pyridin-4-yl)piperidin-3-ylcarbamate (359 mg, 48.5% yield) as a solid.

WORKUP

后处理

  1. temperatureAfter cooling down
  2. concentrationthe residue was concentrated
  3. custompurified by reverse phase chromatography (SP4, 25M, water/ACN 80/20→0/100, 30 CV)