Sulfuric acid magnesium salt (1:1) → HCID 178519077, 화합물

HRID 907842노트

반응식

HRID 907842 반응식
[NH2:1][C:2]1[CH:10]=[C:9]([F:11])[CH:8]=[C:7]2[C:3]=1[CH2:4][O:5][C:6]2=[O:12].[F:13][C:14]1[CH:21]=[CH:20][C:17]([CH:18]=O)=[CH:16][CH:15]=1.[O-]S([O-])(=O)=O.[Mg+2]>C(Cl)Cl>[F:11][C:9]1[CH:8]=[C:7]2[C:3]([CH2:4][O:5][C:6]2=[O:12])=[C:2](/[N:1]=[CH:18]/[C:17]2[CH:20]=[CH:21][C:14]([F:13])=[CH:15][CH:16]=2)[CH:10]=1

참가 물질

5

반응물 3

HCID 24083Sulfuric acid magnesium salt (1:1)HCID 680234-FluorobenzaldehydeHCID 672589744-Amino-6-fluoroisobenzofuran-1(3H)-one

생성물 1

HCID 178519077HCID 178519077, 화합물수율 34.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

4-amino-6-fluoroisobenzofuran-1(3H)-one (1.5 g, 8.98 mmol), 4-fluorobenzaldehyde (1.67 g, 13.47 mmol) and 12.75 g of MgSO4 were added into 40 ml of DCM and stirred under reflux overnight, then the mixture was evaporated under reduced pressure and the residues was dried in vacuum. 850 mg of (E)-6-fluoro-4-(4-fluorobenzylideneamino)isobenzofuran-1(3H)-one was obtained. 1H-NMR (400 MHz, CDCl3) δ (ppm): 5.37 (s, 2); 7.09-7.12 (dd, 1H), 7.19-7.23 (t, 2H), 7.43-7.45 (dd, 1H), 7.92-7.95 (m, 2H), 8.49 (s, 1H); LC-MS (ESI) m/z: 274 (M+1)+.

후처리

  1. temperatureunder reflux overnight
  2. customthe mixture was evaporated under reduced pressure
  3. customthe residues was dried in vacuum

출처 및 근거

ORD 기록
ord-d513d0e3ecfe43c4b4c47c72747ae0dc
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08012976B2

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