Methanol → HCID 86649400, 화합물

HRID 80154

반응식

HRID 80154 반응식
[CH3:1][O:2][NH2:3].C([O-])([O-])=O.[K+].[K+].[F:10][C:11]1[CH:18]=[C:17]([N:19]2[CH2:23][CH2:22][N:21]([C:24]3[CH:25]=[N:26][CH:27]=[CH:28][C:29]=3[CH3:30])[C:20]2=[O:31])[CH:16]=[CH:15][C:12]=1[CH:13]=O.CO>C(COC)OC.C(Cl)(Cl)Cl>[CH3:1][O:2][N:3]=[CH:13][C:12]1[CH:15]=[CH:16][C:17]([N:19]2[CH2:23][CH2:22][N:21]([C:24]3[CH:25]=[N:26][CH:27]=[CH:28][C:29]=3[CH3:30])[C:20]2=[O:31])=[CH:18][C:11]=1[F:10]

참가 물질

7

반응물 4

HCID 887MethanolHCID 4113O-MethylhydroxylamineHCID 11430Potassium CarbonateHCID 596361642-Fluoro-4-[3-(4-methyl-pyridin-3-yl)-2-oxo-imidazolidin-1-yl]-benzaldehyde

생성물 1

HCID 86649400HCID 86649400, 화합물수율 9.1%

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 80711,2-Dimethoxyethane용매

반응 조건

온도
40 °C

실험 절차

O-Methyl-hydroxylamine (84 mg, 1.003 mmol) and K2CO3 (207 mg, 1.5 mmol) were added to a solution of 2-fluoro-4-[3-(4-methyl-pyridin-3-yl)-2-oxo-imidazolidin-1-yl]-benzaldehyde-(I-121a: 300 mg, 1.003 mmol) in dimethoxyethane (10 mL). The resulting mixture was heated to 40° C. for 2 hours. The reaction was monitored by TLC (5% MeOH in CHCl3). The reaction mixture was filtered, washed with CHCl3 and the filtrate was concentrated under reduced pressure to afford 30 mg of crude 2-Fluoro-4-[3-(4-methyl-pyridin-3-yl)-2-oxo-imidazolidin-1-yl]-benzaldehyde O-methyl-oxime, which was used in the next step without further purification.

후처리

  1. filtrationThe reaction mixture was filtered
  2. washwashed with CHCl3
  3. concentrationthe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-faec1e1876794e68b942d7f8dbe08414
출처 데이터셋
uspto-grants-2014_09
특허 번호
USRE045173E1

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