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Trifluoromethanesulfonic anhydride → Ethyl 2-ethoxy-4'-fluoro-6-(((trifluoromethyl)sulfonyl)oxy)biphenyl-4-carboxylate

HRID 530976
ノート
印刷プレビュー

反応式

HRID 530976 の反応式
FC(F)(F)S([O:6][S:7]([C:10]([F:13])([F:12])[F:11])(=[O:9])=[O:8])(=O)=O.[CH2:16]([O:18][C:19]1[CH:24]=[C:23]([C:25]([O:27][CH2:28][CH3:29])=[O:26])[CH:22]=[C:21](O)[C:20]=1[C:31]1[CH:36]=[CH:35][C:34]([F:37])=[CH:33][CH:32]=1)[CH3:17]>N1C=CC=CC=1>[CH2:16]([O:18][C:19]1[CH:24]=[C:23]([C:25]([O:27][CH2:28][CH3:29])=[O:26])[CH:22]=[C:21]([O:6][S:7]([C:10]([F:11])([F:12])[F:13])(=[O:8])=[O:9])[C:20]=1[C:31]1[CH:36]=[CH:35][C:34]([F:37])=[CH:33][CH:32]=1)[CH3:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 67749Trifluoromethanesulfonic anhydrideHCID 90423930Ethyl 2-ethoxy-4'-fluoro-6-hydroxybiphenyl-4-carboxylate

生成物 1

HCID 117992433Ethyl 2-ethoxy-4'-fluoro-6-(((trifluoromethyl)sulfonyl)oxy)biphenyl-4-carboxylate

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

Trifluoromethanesulfonic anhydride (8.66 mL) was added at 0° C. to a mixture of ethyl 2-ethoxy-4′-fluoro-6-hydroxybiphenyl-4-carboxylate (13.0 g) and pyridine (80 mL), and the resultant mixture was stirred at the same temperature as above for 20 minutes. The reaction mixture was passed through a short silica gel (NH) column, and the solvent was distilled off under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate) to obtain the title compound (15.6 g).

後処理

  1. distillationthe solvent was distilled off under reduced pressure
  2. customThe obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate)

出典と根拠

ORDレコード
ord-4b69b4ce59544614ade2e82a8299df26
出典データセット
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09353108B2

反応ノート

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