HRID38904

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID79081

3-Methylpiperidine

C6H13N

结构：Cc1ccc(S(=O)(=O)OC[C@@H]2COc3ccc(S(C)(=O)=O)cc3O2)cc1

HCID86652934

未命名化合物

PRODUCTS

生成物

结构：CC1CCCN(C[C@@H]2COc3ccc(S(C)(=O)=O)cc3O2)C1

HCID44469458

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID6342

Acetonitrile

C2H3N

CONDITIONS

反应条件

温度: 120 °C

PROCEDURE

实验过程

A mixture of [(2S)-7-(methylsulfonyl)-2,3-dihydro-1,4-benzodioxin-2-yl]methyl 4-methylbenzenesulfonate (0.20 g, 0.5 mmol), 3-methylpiperidine (0.35 ml, 3 mmol) and ACN (2 ml) was heated under microwave radiation at 120° C. for 30 min. Purification on flash column chromatography (Isooctane/EtOAc/MeOH). Yield: 0.097 g, 85%. The amine was converted to the fumaric acid salt and crystallized from MeOH/(i-Pr)2O. M.p. 159° C. MS m/z (rel. intensity, 70 eV) 325 (M+, 1), 113 (83), 112 (bp), 69 (43), 55 (46). [α]=+50° (MeOH).

WORKUP

后处理

customPurification on flash column chromatography (Isooctane/EtOAc/MeOH)
customcrystallized from MeOH/(i-Pr)2O
custom[α]=+50° (MeOH)