反応 #324397

ord-0b2fd4e5ef0a43adaa134212b9214a56

反応方程式

CC(C)(C)[Si](C)(C)Oc1ccc(CC(=O)O)cc1
2-[4-(tert-butyldimethylsilyloxy)phenyl]acetic acid
O=C(Cl)C(=O)Cl
oxalyl dichloride
CC(C)(C)[Si](C)(C)Oc1ccc(CC(=O)Cl)cc1
2-[4-(tert-butyldimethylsilyloxy)phenyl]acetyl chloride

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他while elevating to room temperature
  2. 2
    濃縮The mixture was concentrated under reduced pressure

実験手順

Under an argon atmosphere, to a solution of 2-[4-(tert-butyldimethylsilyloxy)phenyl]acetic acid (9) (757 mg, 2.84 mmol) in CH2Cl2 (8 mL) was added DMF (2 drops) by a Pasteur pipette at room temperature. To this was added oxalyl dichloride (490 μL, 5.79 mmol) at 0° C. and the mixture was stirred for 30 minutes while elevating to room temperature. The mixture was concentrated under reduced pressure to give crude 2-[4-(tert-butyldimethylsilyloxy)phenyl]acetyl chloride (10) as a colorless oil, which was used in the following reaction without further purification.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08642281B2uspto-grants-2014_02