Pyridine, hydrofluoride (1:1) → HCID 68814399, 화합물

HRID 732542노트

반응식

HRID 732542 반응식
[F:1][B-](F)(F)F.N#[O+].N1C=CC=CC=1.[FH:14].[CH3:15][O:16][C:17](=[O:43])[C:18]1[CH:30]=[C:29]([C:31]2([C:37]3[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=3)SCCCS2)[CH:28]=[C:20]([C:21]([N:23]([CH3:27])[CH2:24][CH2:25][CH3:26])=[O:22])[CH:19]=1>ClCCl>[CH3:15][O:16][C:17](=[O:43])[C:18]1[CH:30]=[C:29]([C:31]([F:1])([F:14])[C:37]2[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=2)[CH:28]=[C:20]([C:21]([N:23]([CH3:27])[CH2:24][CH2:25][CH3:26])=[O:22])[CH:19]=1

참가 물질

5

반응물 3

HCID 64774Pyridine, hydrofluoride (1:1)HCID 11137142Nitrilooxonium tetrafluoroborateHCID 86615014HCID 86615014, 화합물

생성물 1

HCID 68814399HCID 68814399, 화합물수율 42%

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

실험 절차

Chill a solution of nitrosonium tetrafluoroborate (0.074 g, 0.63 mmol), hydrogen fluoride-pyridine (0.250 mL) in dichloromethane (2 mL) in aplastic bottle. Add a solution of N-methyl-5-(2-phenyl-[1,3]dithian-2-yl)-N-propyl-isophthalamic acid methyl ester (0.123 g, 0.286 mmol) in dichloromethane (1 mL) to the bottle and stir at room temperature for 2 h. Dilute the solution with dichloromethane (5 mL) and filter though a pad of magnesium sulfate and aluminum oxide. Wash solid with ethyl acetate (50 mL), concentrate and purify (silica gel chromatography, eluting with 20:80 to 30:70 ethyl acetate:hexanes) to give the title compound (42%).

후처리

  1. filtrationfilter though a pad of magnesium sulfate and aluminum oxide
  2. washWash solid with ethyl acetate (50 mL)
  3. concentrationconcentrate
  4. custompurify
  5. wash(silica gel chromatography, eluting with 20:80 to 30:70 ethyl acetate:hexanes)

출처 및 근거

ORD 기록
ord-cd8d50f666e34d2190c3c44100c4cf65
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07585885B2

반응 노트

불러오는 중…