反应 #66022

ord-a06dae072eb2430396e7a4c03ad82404

反应方程式

CC(C)(C)OC(=O)CN(CC(=O)OC(C)(C)C)S(=O)(=O)c1ccc(Oc2ccccc2)cc1
Compound 4a
CC(C)(C)OC(=O)CN(CC(=O)OC(C)(C)C)S(=O)(=O)c1ccc(Oc2ccccc2)cc1
{[4-Phenoxy-benzenesulphonyl]-tert-butoxycarbonylmethyl-amino}-aceticacid tert-butyl ester
O=C(O)CN(CC(=O)O)S(=O)(=O)c1ccc(Oc2ccccc2)cc1
{[4-Phenoxy-benzenesulphonyl]-carboxymethyl-amino}-acetic acid

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤The solid was filtered off
  2. 2
    其他the filtrate was evaporated in vacuo
  3. 3
    其他The pure product obtained
  4. 4
    其他was dried overnight in high vacuum

实验过程

Compound 4a (1.02 g, 2.14 mmol) was dissolved in formic acid (10 mL) and stirred overnight at room temperature. The solid was filtered off, the filtrate was evaporated in vacuo, and co-evaporated with toluene (6×20 mL). The pure product obtained was dried overnight in high vacuum. Yield: 0.71 g, 1.95 mmol, 91% (off-white solid). 1H-NMR (DMSO-d6): δ 7.91 (d, 2H, 3JHH=9.0 Hz, ArH), 7.20 (d, 2H, 3JHH=9.0 Hz, ArH), 7.28 (d, 2H, 3JHH=9.0 Hz, ArH), 7.00 (d, 1H, 3JHH=9.0 Hz, ArH), 6.87 (d, 2H, 3JHH=9.0 Hz, ArH), 4.07 (s, 4H, 2×CH2CO2H).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08524194B2uspto-grants-2013_09