Hydroxyamine hydrochloride → HCID 58442360, 화합물

HRID 887841노트

반응식

HRID 887841 반응식
[F:1][C:2]([F:29])([F:28])[CH:3]([OH:27])[CH2:4][NH:5][C:6]([C:8]1[C:13]([N:14]2C(C)=CC=C2C)=[CH:12][C:11]([C:21]([F:24])([F:23])[F:22])=[C:10]([O:25][CH3:26])[N:9]=1)=[O:7].Cl.NO>CCO.O>[F:29][C:2]([F:1])([F:28])[CH:3]([OH:27])[CH2:4][NH:5][C:6]([C:8]1[C:13]([NH2:14])=[CH:12][C:11]([C:21]([F:22])([F:24])[F:23])=[C:10]([O:25][CH3:26])[N:9]=1)=[O:7]

참가 물질

5

반응물 2

HCID 443297Hydroxyamine hydrochlorideHCID 866576653-(2,5-Dimethyl-pyrrol-1-yl)-6-methoxy-5-trifluoromethyl-pyridine-2-carboxylic acid (3,3,3-trifluoro-2-hydroxy-propyl)-amide

생성물 1

HCID 58442360HCID 58442360, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

3-(2,5-Dimethyl-pyrrol-1-yl)-6-methoxy-5-trifluoromethyl-pyridine-2-carboxylic acid (3,3,3-trifluoro-2-hydroxy-propyl)-amide (350 mg, 0.823 mmol) was dissolved in EtOH (14 ml) and water (7 ml). Hyroxylamine hydrochloride (572 mg, 8.23 mmol) was added followed by TEA (167 mg, 1.646 mmol) and the mixture was heated at reflux overnight. After cooling the RT, the mixture was purified by reverse phase chromatography eluting with MeOH; water (0.1% TFA) to afford the title compound as a pale yellow solid; LC-MS Rt=4.20 min[M+H]+ 348.2 (Method 10minLC_v002)

후처리

  1. temperaturethe mixture was heated
  2. temperatureat reflux overnight
  3. customthe mixture was purified by reverse phase chromatography
  4. washeluting with MeOH

출처 및 근거

ORD 기록
ord-c012ff92bdae4a6e89c9b38ac7e20773
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08247436B2

반응 노트

불러오는 중…