HRID424592

反应详情

EQUATION

反应方程式

HRID 424592 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-(4-(Pyrrolidin-3-yl)-3,4-dihydro-2H-benzo[b][1,4]thiazin-7-yl)thiophene-2-carboximidamide (0.1264 g, 0.367 mmol) in MeOH (3 mL) was treated with 1M HCl in ether (1.835 mL, 1.835 mmol). The mixture was stirred at room temperature for 5 minutes and was concentrated to give a light yellow solid (0.16 g, quantitative). 1H NMR (DMSO-d6) δ 11.30 (s, 1H), 9.83 (brs, 1H), 9.70 (s, 1H), 9.57 (brs, 1H), 8.70 (s, 1H), 8.15-8.13 (m, 2H), 7.37-7.34 (m, 1H), 7.10-7.00 (m, 3H), 4.74-4.63 (m, 1H), 3.60-3.40 (m, 5H), 3.16-3.05 (m, 3H), 2.26-2.15 (m, 1H), 2.05-1.92 (m, 1H); ESI-MS (m/z, %): 347, 345 (MH+, freebase, 61), 278, 276 (100); HRMS (C17H21N4S2, MH+, freebase): calculated: 345.1202, observed: 345.1195. HPLC purity: 99% by area.

WORKUP

后处理

  1. concentrationwas concentrated
  2. customto give a light yellow solid (0.16 g, quantitative)