反应 #2267081

ord-fef2f01eefd34a739a8096f360924edc

反应方程式

O
Water
COc1ccc(CC(C)O)c(C(=NNC(C)=O)c2ccc([N+](=O)[O-])cc2)c1NC(C)=O
23
COc1ccc(CC(C)O)c(C(=NNC(C)=O)c2ccc([N+](=O)[O-])cc2)c1NC(C)=O
2′-Acetylamino-6′-(2-hydroxypropyl)-3′-methoxy-4-nitrobenzophenone acetylhydrazone
CCN(CC)CC
triethyl amine
CS(=O)(=O)Cl
methanesulfonyl chloride
COc1ccc(CC(C)OS(C)(=O)=O)c(C(=NNC(C)=O)c2ccc([N+](=O)[O-])cc2)c1NC(C)=O
product 24
COc1ccc(CC(C)OS(C)(=O)=O)c(C(=NNC(C)=O)c2ccc([N+](=O)[O-])cc2)c1NC(C)=O
2′-Acetylamino-6′-(2-methanesulfonyloxypropyl)-3′-methoxy-4-nitrobenzophenone acetylhydrazone

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    萃取extracted with CH2Cl2
  2. 2
    洗涤The organic phase was washed with HCl (1N), brine
  3. 3
    干燥dried over Na2SO4
  4. 4
    其他Removal of the solvent

实验过程

To a solution of 23 (1.1 g) in 20 ml of CH2Cl2 was added 1.5 ml of triethyl amine, 0.60 ml of methanesulfonyl chloride at 0-10° C. After 30 min, no more starting material was detected on TLC. Water was added, extracted with CH2Cl2. The organic phase was washed with HCl (1N), brine, dried over Na2SO4. Removal of the solvent afforded product 24 (1.21 g).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06887867B2uspto-grants-2005_05