反応 #2358516

ord-98903a7157c04e8bafdaf51c9456d308

反応方程式

CS(=O)(=O)c1cc(F)cc(OCCBr)c1
1-(2-bromoethoxy)-3-fluoro-5-methylsulfonyl-benzene
CCNCC
di-ethylamine
CCN(CC)CCOc1cc(F)cc(S(C)(=O)=O)c1
title compound
収率 61.7%
CCN(CC)CCOc1cc(F)cc(S(C)(=O)=O)c1
N,N-diethyl-2-(3-fluoro-5-methylsulfonyl-phenoxy)ethanamine
収率 61.7%

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他Preparation
  2. 2
    その他Purification by flash column chromatography (ethyl acetate/methanol, 1:0 to 1:1)

実験手順

Preparation according to Example 1 but performed in one portion: 1-(2-bromoethoxy)-3-fluoro-5-methylsulfonyl-benzene (0.5 g, 1.68 mmol) and di-ethylamine (1.39 ml, 13.46 mmol) in ethanol (4 ml). Purification by flash column chromatography (ethyl acetate/methanol, 1:0 to 1:1) gave the title compound (300 mg, 61.6%). The amine was converted to the hydrochloric acid salt and re-crystallized from methanol/diethyl ether: M.p. 172.3° C. MS m/z (relative intensity, 70 eV) 289 (M+, 1), 274 (6), 87 (6), 86 (bp), 58 (5).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09120728B2uspto-grants-2015_09