反応 #57669

反応方程式

5,7-dichloro-4-methoxy-3-methyl-benzofuran-2-carboxylic acid

(S)-2-(4′-amino-biphenyl-4-sulfonylamino)-3-methyl-butyric acid tert-butyl ester

BOP

N,N-diisopropylethylamine

→

(S)-2-{4′-[(5,7-dichloro-4-methoxy-3-methyl-benzofuran-2-carbonyl)-amino]-biphenyl-4-sulfonylamino}-3-methyl-butyric acid tert-butyl ester

収率 60.0%

溶媒

DMF

反応条件

後処理

1. 1
   洗浄The mixture was washed with brine
2. 2
   抽出was extracted with ethyl acetate
3. 3
   洗浄The combined ethyl acetate layers were washed with brine
4. 4
   その他Removal of the solvent
5. 5
   その他in vacuo and purification of the residue by column chromatography on silica gel

実験手順

To 80 mg of 5,7-dichloro-4-methoxy-3-methyl-benzofuran-2-carboxylic acid was added 120 mg of (S)-2-(4′-amino-biphenyl-4-sulfonylamino)-3-methyl-butyric acid tert-butyl ester, 154 mg of BOP, 50 mg of N,N-diisopropylethylamine and 4 mL of DMF. The mixture was stirred at room temperature for 48 h. The mixture was washed with brine and was extracted with ethyl acetate. The combined ethyl acetate layers were washed with brine. Removal of the solvent in vacuo and purification of the residue by column chromatography on silica gel gave 110 mg (60% yield) of (S)-2-{4′-[(5,7-dichloro-4-methoxy-3-methyl-benzofuran-2-carbonyl)-amino]-biphenyl-4-sulfonylamino}-3-methyl-butyric acid tert-butyl ester as an off-white solid.

出典