HRID570598
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- waitThe reaction was left at 0° C. for 15 minutes
- customThe solid precipitated
- filtrationwas filtered
- washwashed several times with water until the pH of the filtrate
- dry with materialThe white solid (1.4 g, 98%) was dried in the Buchner funnel
- customused immediately for the next reaction