反応 #1994313

ord-4eb56d03af454cff85c6a47a66e96a2b

反応方程式

CCN(C(C)C)C(C)C
DIPEA
CC(C)(C)OC(=O)N[C@@H](CCCNC(=N)N)C(=O)O
Boc-Arg-OH
c1ccc(CNCc2ccccc2)cc1
NH(CH2Ph)2
Cl[P+](N1CCCC1)(N1CCCC1)N1CCCC1.F[P-](F)(F)(F)(F)F
PyCloP
CC(C)(C)OC(=O)N[C@@H](CCCNC(=N)N)C(=O)N(Cc1ccccc1)Cc1ccccc1
Boc-Arg-N(CH2Ph)2

試薬

なし

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONwas added
  2. 2
    workup.STIRRINGThe solution was stirred for 1 h at room temperature
  3. 3
    その他The reaction mixture was evaporated
  4. 4
    workup.DISSOLUTIONredissolved in ethyl acetate
  5. 5
    洗浄washed with citric acid, sodium bicarbonate and brine
  6. 6
    その他The solvent was removed under vacuum

実験手順

A solution of Boc-Arg-OH(1 eq), NH(CH2Ph)2 (1.1 eq) and PyCloP (1 eq) in dry DCM (filtered through alumina) (2 ml) and DMF (1 ml). The solution was cooled on ice and DIPEA (2 eq) was added under stirring. The solution was stirred for 1 h at room temperature. The reaction mixture was evaporated, and redissolved in ethyl acetate and washed with citric acid, sodium bicarbonate and brine. The solvent was removed under vacuum and the Boc protecting group of the resulting peptide was deprotected in the dark using 95% TFA.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08598114B2uspto-grants-2013_12