反応 #66022

ord-a06dae072eb2430396e7a4c03ad82404

反応方程式

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

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

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

実験手順

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).

出典

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