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HRID20480

反应详情

EQUATION

反应方程式

HRID 20480 的结构方程式

REACTANTS

反应物

2
结构：COCC(=O)Cl
HCID96623

Acetyl chloride, methoxy-

C3H5ClO2

结构：C[C@@H]1NC([C@@H](O)[C@@H](N)Cc2cc(F)cc(F)c2)CO[C@H]1OCC(C)(C)C
HCID68563960

未命名化合物

PRODUCTS

生成物

1
结构：COCC(=O)N[C@@H](Cc1cc(F)cc(F)c1)[C@H](O)[C@H]1CO[C@@H](OCC(C)(C)C)[C@H](C)N1.Cl
HCID68560724

未命名化合物

收率 65.1%

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Dissolve (1S,2S)-2-amino-3-(3,5-difluorophenyl)-1-[(5S,6R)-6-(2,2-dimethylpropoxy)-5-methylmorpholin-3-yl]-propan-1-ol (31 mg, 0.083 mmol) in dry 1:1 dichloromethane:diethyl ether (1 mL) under nitrogen. Cool to 0° C. and add dropwise methoxyacetyl chloride (7.6 μL, 0.083 mmol). Stir for 1 hour, quench with methanol, concentrate and purify (reverse-phase HPLC, eluting with 10:90 to 50:50 acetonitrile:water with 8 mM hydrochloric acid), to give the title compound (26 mg, 65%).

WORKUP

后处理

  1. dry with materialin dry 1:1 dichloromethane
  2. customquench with methanol
  3. concentrationconcentrate
  4. custompurify
  5. wash(reverse-phase HPLC, eluting with 10:90 to 50:50 acetonitrile:water with 8 mM hydrochloric acid)