反応 #41991

反応方程式

3-(1-ethyl-5-fluoro-indan-1-yl)-1H-indol-7-ylamine

methyl chloroformate

→

title compound

収率 36.0%

[3-(1-Ethyl-5-fluoro-indan-1-yl)-1H-indol-7-yl]-carbamic acid methyl ester

収率 36.0%

溶媒

ether

pyridine

反応条件

後処理

1. 1
   洗浄wash with 1N aqueous hydrochloric acid (2×)
2. 2
   乾燥dry over anhydrous sodium sulfate
3. 3
   ろ過filter
4. 4
   濃縮concentrate solution in vacuo
5. 5
   その他Purify the residue on silica eluting with 0 to 75% ethyl acetate/hexanes over 30 minutes

実験手順

Dissolve 3-(1-ethyl-5-fluoro-indan-1-yl)-1H-indol-7-ylamine (0.35 g, 1.19 mmol) in pyridine (3 ml). Add methyl chloroformate (0.10 ml, 1.31 mmol, 1.1 equivalents) and stir at room temperature under nitrogen overnight. Dilute with ether, wash with 1N aqueous hydrochloric acid (2×), dry over anhydrous sodium sulfate, filter, and concentrate solution in vacuo. Purify the residue on silica eluting with 0 to 75% ethyl acetate/hexanes over 30 minutes to provide the title compound as a white solid (0.15 g, 36%). LC-MS m/z 353.1 (M++1).

出典