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HRID1747154

反应详情

EQUATION

反应方程式

HRID 1747154 的结构方程式

REACTANTS

反应物

3
结构：C=O
HCID712

Formaldehyde

CH2O

结构：Cc1ccc(S(=O)(=O)O)cc1.O
HCID521998

4-Methylbenzenesulfonic acid hydrate

C7H10O4S

结构：O=C1c2ccccc2C(=O)N1[C@@H]1C[C@H]2OCC[C@@]2(C(=O)NCc2cc(C(F)(F)F)ccc2O)C1
HCID86708154

未命名化合物

PRODUCTS

生成物

1
结构：O=C1c2ccccc2C(=O)N1[C@@H]1C[C@H]2OCC[C@@]2(C(=O)N2COc3ccc(C(F)(F)F)cc3C2)C1
HCID86708155

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：Cc1ccccc1
溶剂HCID1140

Toluene

C7H8

PROCEDURE

实验过程

A solution of the product of Step C (7.97 g, 15.5 mmol, 1 eq), paraformaldehyde (9.28 g, 310 mmol, 20 eq) and p-toluenesulfonic acid hydrate (2.94 g, 15.5 mmol, 1 eq) in toluene (300 mL) was heated to 130° C. for 18 hours in a flask equipped with a Dean-Stark trap. The solution was cooled to rt and concentrated. Purification by chromatography (200 g column) eluting with 25 to 60 to 100% ethyl acetate/heptane afforded the product of Step D. Calculated for C25H21F3N2O5: 487.1 (M+1). found: 487.2.

WORKUP

后处理

  1. customequipped with a Dean-Stark trap
  2. concentrationconcentrated
  3. customPurification by chromatography (200 g column)
  4. washeluting with 25 to 60 to 100% ethyl acetate/heptane