HRID570598

反应详情

EQUATION

反应方程式

HRID 570598 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To the solid product N-(tert.-butoxycarbonyl)-O-(mesitylsulfonyl)-hydroxylamine (2.1 g, 6.6 mmol) was added trifluoroacetic acid (20 mL) slowly at 0° C. under a nitrogen atmosphere. The reaction mixture was stirred for 30 minutes followed slowly by water (60 mL). The reaction was left at 0° C. for 15 minutes. The solid precipitated was filtered and washed several times with water until the pH of the filtrate was neutral. The white solid (1.4 g, 98%) was dried in the Buchner funnel and used immediately for the next reaction; 1H NMR (400 MHz, DMSO-d6): δ 6.73 (s, 2H), 2.48 (s, 6H), 2.15 (s, 3H).

WORKUP

后处理

  1. waitThe reaction was left at 0° C. for 15 minutes
  2. customThe solid precipitated
  3. filtrationwas filtered
  4. washwashed several times with water until the pH of the filtrate
  5. dry with materialThe white solid (1.4 g, 98%) was dried in the Buchner funnel
  6. customused immediately for the next reaction