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Trifluoroacetic acid → 3-(6'-Methyl-6''-trifluoromethyl-[2,2';4',3'']terpyridin-6-yl)-benzenesulfonamide

HRID 906301
ノート
印刷プレビュー

反応式

HRID 906301 の反応式
C([NH:5][S:6]([C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([C:15]2[N:20]=[C:19]([C:21]3[CH:26]=[C:25]([C:27]4[CH:28]=[N:29][C:30]([C:33]([F:36])([F:35])[F:34])=[CH:31][CH:32]=4)[CH:24]=[C:23]([CH3:37])[N:22]=3)[CH:18]=[CH:17][CH:16]=2)[CH:10]=1)(=[O:8])=[O:7])(C)(C)C.C(O)(C(F)(F)F)=O>>[CH3:37][C:23]1[N:22]=[C:21]([C:19]2[CH:18]=[CH:17][CH:16]=[C:15]([C:11]3[CH:10]=[C:9]([S:6]([NH2:5])(=[O:8])=[O:7])[CH:14]=[CH:13][CH:12]=3)[N:20]=2)[CH:26]=[C:25]([C:27]2[CH:28]=[N:29][C:30]([C:33]([F:35])([F:34])[F:36])=[CH:31][CH:32]=2)[CH:24]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 6422Trifluoroacetic acidHCID 67392744HCID 67392744、化合物

生成物 1

HCID 673939233-(6'-Methyl-6''-trifluoromethyl-[2,2';4',3'']terpyridin-6-yl)-benzenesulfonamide収率 48%

反応条件

温度
23 °C

実験手順

To N-tert-butyl-3-(6′-methyl-6″-trifluoromethyl-[2,2′;4′,3″]terpyridin-6-yl)-benzenesulfonamide (Example 29) (0.075 g, 0.142 mmol) was added TFA (2 mL) and the reaction mixture was stirred at 23° C. for 16 h. The mixture was partitioned between EtOAc and saturated NaHCO3 solution, the organic layer was dried over Na2SO4. Removal of the solvent in vacuum left a crude product which was triturated with diethyl ether to give the title compound as an off-white solid (0.032 g, 48%). MS (ISP) 471.0 [(M+H)+]; mp 233-234° C.

後処理

  1. customThe mixture was partitioned between EtOAc and saturated NaHCO3 solution
  2. dry with materialthe organic layer was dried over Na2SO4
  3. customRemoval of the solvent in vacuum
  4. waitleft a crude product which
  5. customwas triturated with diethyl ether

出典と根拠

ORDレコード
ord-dd4dbb29cb49433c8831d77dfe7c0087
出典データセット
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08012986B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート