Chloroform → HCID 68521334, 화합물

HRID 2384520노트

반응식

HRID 2384520 반응식
[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

참가 물질

5

반응물 2

HCID 6212ChloroformHCID 68519824HCID 68519824, 화합물

생성물 1

HCID 68521334HCID 68521334, 화합물

시약·촉매·용매 2

HCID 23925Iron촉매HCID 176Acetic Acid용매

반응 조건

온도
65 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5447f3b459614853822be6549a6b67cc
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08263773B2

반응 노트

불러오는 중…