Sodium Hydroxide → HCID 117940033, 화합물

HRID 62284노트

반응식

HRID 62284 반응식
[CH3:1][O:2][C:3]1[CH:11]=[C:10]2[C:6]([CH2:7][CH2:8][C:9]2=[O:12])=[CH:5][C:4]=1[N:13]1[CH2:18][CH2:17][O:16][CH2:15][CH2:14]1.CO.O.[F:22][C:23]([F:39])([F:38])[C:24]([C:30]1[CH:31]=[N:32][CH:33]=[C:34]([CH:37]=1)[CH:35]=O)([OH:29])[C:25]([F:28])([F:27])[F:26].[OH-].[Na+]>C(Cl)(Cl)Cl>[F:28][C:25]([F:26])([F:27])[C:24]([C:30]1[CH:37]=[C:34](/[CH:35]=[C:8]2/[C:9](=[O:12])[C:10]3[C:6]([CH2:7]/2)=[CH:5][C:4]([N:13]2[CH2:14][CH2:15][O:16][CH2:17][CH2:18]2)=[C:3]([O:2][CH3:1])[CH:11]=3)[CH:33]=[N:32][CH:31]=1)([OH:29])[C:23]([F:39])([F:38])[F:22]

참가 물질

6

반응물 4

HCID 14798Sodium HydroxideHCID 177581373-Pyridinecarboxaldehyde, 5-[2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl]-HCID 22242641Methanol--water (1/1)HCID 1179401286-Methoxy-5-morpholino-2,3-dihydro-1H-inden-1-one

생성물 1

HCID 117940033HCID 117940033, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

To a solution of 13 (0.1 g, 0.40 mmol)), MeOH/H2O (1:1), was added 5-(1,1,1,3,3,3-hexafluoro-2-hydroxypropan-2-yl)nicotinaldehyde 259 (0.132 g, 0.485 mmol) and NaOH (0.032 g, 0.80 mmol). The reaction was stirred at RT for 6 h. The reaction mass was diluted with chloroform and washed with water (3×25 ml). The organic layer was dried over sodium sulphate and concentrated to get the crude 263, which was purified through flash chromatography by using 100-200 mesh silica gel. The compound was eluted at 30% ethyl acetate in hexane to afford yellow coloured solid (E)-2-((5-(1,1,1,3,3,3-hexafluoro-2-hydroxypropan-2-yl)pyridin-3-yl)methylene)-6-methoxy-5-morpholino-2,3-dihydro-1H-inden-1-one 263.

후처리

  1. washwashed with water (3×25 ml)
  2. dry with materialThe organic layer was dried over sodium sulphate
  3. concentrationconcentrated
  4. customto get the crude 263, which
  5. customwas purified through flash chromatography
  6. washThe compound was eluted at 30% ethyl acetate in hexane

출처 및 근거

ORD 기록
ord-19b8e5b3de1d45c78f0b4c8371ecb9a4
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09446047B2

반응 노트

불러오는 중…