Tetrahydrofuran → HCID 66810488, 화합물

HRID 455241노트

반응식

HRID 455241 반응식
[C:1]([C:3]1[CH:30]=[C:29]([N+:31]([O-])=O)[CH:28]=[CH:27][C:4]=1[O:5][C:6]1[CH:7]=[CH:8][C:9]([F:26])=[C:10]([NH:12][C:13](=[O:25])[CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([C:21]([F:24])([F:23])[F:22])[CH:16]=2)[CH:11]=1)#[N:2].O1CCCC1>C(O)C.[C].[Pd]>[NH2:31][C:29]1[CH:28]=[CH:27][C:4]([O:5][C:6]2[CH:7]=[CH:8][C:9]([F:26])=[C:10]([NH:12][C:13](=[O:25])[CH2:14][C:15]3[CH:20]=[CH:19][CH:18]=[C:17]([C:21]([F:22])([F:23])[F:24])[CH:16]=3)[CH:11]=2)=[C:3]([C:1]#[N:2])[CH:30]=1

참가 물질

5

반응물 2

HCID 8028TetrahydrofuranHCID 66810481HCID 66810481, 화합물

생성물 1

HCID 66810488HCID 66810488, 화합물수율 92.1%

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 702Ethanol용매

실험 절차

To a solution of N-[5-(2-cyano-4-nitrophenoxy)-2-fluorophenyl]-2-[3-(trifluoromethyl)phenyl]acetamide (1.36 g, 2.96 mmol) in ethanol (25 mL)/tetrahydrofuran (10 mL) was added 10% palladium-carbon (160 mg), and the mixture was stirred at room temperature for 5 hr under a hydrogen atmosphere (1 atm). Insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. The obtained residue was purified by basic silica gel column chromatography (ethyl acetate/n-hexane=30/70→100/0), and the fraction containing the object product was concentrated under reduced pressure to give the title compound (1.17 g, 92%) as a beige amorphous form.

후처리

  1. filtrationInsoluble material was filtered off
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customThe obtained residue was purified by basic silica gel column chromatography (ethyl acetate/n-hexane=30/70→100/0)
  4. additionthe fraction containing the object product
  5. concentrationwas concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-7f2052be77994879a8268927d4649a17
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08497274B2

반응 노트

불러오는 중…