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HRID2224021

反应详情

EQUATION

反应方程式

HRID 2224021 的结构方程式

REACTANTS

反应物

3
结构：CCN(C(C)C)C(C)C
HCID81531

Diisopropylethylamine

C8H19N

结构：CC(C)(C)[Si](C)(C)O[C@@H]1CC[C@H](N)C(=O)N(Cc2cccnc2)C1
HCID69267176

未命名化合物

结构：COC1C(=O)O[C@H]2C1OC(C)(C)O[C@@H]2/C=C/C(C)(C)C
HCID69267460

未命名化合物

PRODUCTS

生成物

1
结构：CO[C@@H](C(=O)N[C@H]1CC[C@@H](O[Si](C)(C)C(C)(C)C)CN(Cc2cccnc2)C1=O)[C@@H]1OC(C)(C)O[C@H](/C=C/C(C)(C)C)[C@H]1O
HCID69266828

未命名化合物

收率 57.2%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CC(C)O
溶剂HCID3776

Isopropanol

C3H8O

PROCEDURE

实验过程

A solution of (3S,6R)-3-amino-6-(tert-butyl-dimethyl-silanyloxy)-1-pyridin-3-ylmethyl-azepan-2-one (1.84 g, 5.3 mmol), (4R,4aR)-4-((E)-3,3-Dimethyl-but-1-enyl)-7-methoxy-2,2-dimethyl-tetrahydro-furo[3,2-d][1,3]dioxin-6-one (1.0 g, 3.5 mmol) and diisopropylethylamine (1.37 g, 11.0 mmol) in isopropanol (10 mL) is refluxed for 16 h. The solution is evaporated and chromatographed on silica (95% CH2Cl2/5% CH3OH) to give 1.27 g (57.0%) of (R)-N-[(3S,6R)-6-(tert-butyl-dimethyl-silanyloxy)2-oxo-1-pyridin-3-ylmethyl-azepan-3-yl]-2-[(4R,5R,6R)-6-((E)-3,3-dimethyl-but-1-enyl)-5-hydroxy-2,2-dimethyl-[1,3]dioxan-4-yl]-2-methoxy-acetamide as a white solid. MS (ESI) 634.3 (M+H)+

WORKUP

后处理

  1. customThe solution is evaporated
  2. customchromatographed on silica (95% CH2Cl2/5% CH3OH)