反应 #324387

ord-1d5259be15ab4b08ac29b9f2208c3096

反应方程式

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

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他while elevating to room temperature
  2. 2
    浓缩The mixture was concentrated under reduced pressure

实验过程

Under an argon atmosphere, to a solution of 2-[4-(tert-butyldimethylsilyloxy)phenyl]acetic acid (9) (2.12 g, 7.96 mmol) in CH2Cl2 (10 mL) was added DMF (3 drops) by a Pasteur pipette at room temperature. To this was added oxalyl dichloride (1.35 mL, 16.0 mmol) at 0° C. and the mixture was stirred for an hour 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.

来源

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