Chloroform → HCID 68521334、化合物

HRID 2384520ノート

反応式

HRID 2384520 の反応式
[Br:1][C:2]1[C:10]2[C:5](=[N+:6]([O-])[CH:7]=[C:8]([N+:11]([O-])=O)[CH:9]=2)[S:4][C:3]=1[S:15]([C:18]1[CH:23]=[C:22]([F:24])[CH:21]=[C:20]([C:25]#[N:26])[CH:19]=1)(=[O:17])=[O:16].C(Cl)(Cl)Cl>C(O)(=O)C.[Fe]>[NH2:11][C:8]1[CH:9]=[C:10]2[C:2]([Br:1])=[C:3]([S:15]([C:18]3[CH:23]=[C:22]([F:24])[CH:21]=[C:20]([C:25]#[N:26])[CH:19]=3)(=[O:16])=[O:17])[S:4][C:5]2=[N:6][CH:7]=1

参加物

5

反応物 2

HCID 6212ChloroformHCID 68519824HCID 68519824、化合物

生成物 1

HCID 68521334HCID 68521334、化合物

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 176Acetic Acid溶媒

反応条件

温度
65 °C

実験手順

3-Bromo-2-(3-cyano-5-fluoro-benzenesulfonyl)-5-nitro-thieno[2,3-b]pyridin-N-oxide (1.0 g, 2.18 mmol) was suspended in acetic acid (12 ml) and Fe powder was added (0.73 g, 13 mmol). The reaction mixture was stirred at 60-70° C. for 60 minutes. Chloroform (45 ml) was added and after filtration through celite the filtrate was evaporated, the crude residue was treated with methanol (3 ml). The product was filtered, washed with methanol. It was obtained (0.69 g, 76.7%) as a yellow powder. LC-MS: (M+H)+ 413.1.

後処理

  1. filtrationafter filtration through celite the filtrate
  2. customwas evaporated
  3. additionthe crude residue was treated with methanol (3 ml)
  4. filtrationThe product was filtered
  5. washwashed with methanol
  6. customIt was obtained (0.69 g, 76.7%) as a yellow powder

出典と根拠

ORDレコード
ord-5447f3b459614853822be6549a6b67cc
出典データセット
uspto-grants-2012_09
特許番号
US08263773B2

反応ノート

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