Sulfuric acid magnesium salt (1:1) → HCID 178484438, 화합물

HRID 1467650노트

반응식

HRID 1467650 반응식
[NH2:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]2[C:3]=1[CH2:4][O:5][C:6]2=[O:11].[CH:12]([C:14]1[CH:24]=[CH:23][C:17]([C:18]([N:20]([CH3:22])[CH3:21])=[O:19])=[CH:16][CH:15]=1)=O.[O-]S([O-])(=O)=O.[Mg+2]>C(#N)C>[CH3:22][N:20]([CH3:21])[C:18](=[O:19])[C:17]1[CH:23]=[CH:24][C:14](/[CH:12]=[N:1]/[C:2]2[CH:10]=[CH:9][CH:8]=[C:7]3[C:3]=2[CH2:4][O:5][C:6]3=[O:11])=[CH:15][CH:16]=1

참가 물질

5

반응물 3

HCID 24083Sulfuric acid magnesium salt (1:1)HCID 105592054-formyl-N,N-dimethylbenzamideHCID 122846494-Amino-1,3-dihydro-2-benzofuran-1-one

생성물 1

HCID 178484438HCID 178484438, 화합물수율 80.5%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

4-Aminoisobenzofuran-1(3H)-one (2.10 g, 14.1 mmol), 4-formyl-N,N-dimethylbenzamide (2.50 g, 14.1 mmol) and dry MgSO4 (9.84 g, 82 mmol) were added to acetonitrile (170 mL) and stirred under reflux overnight. The mixture was filtered, and the solvent was evaporated under reduced pressure and the residue was re-crystallized to obtain 3.5 g of title compound as a pale solid. 1H-NMR (400 MHz, CDCl3) δ (ppm): 3.01 (s, 3H), 3.15 (s, 3H), 5.43 (s, 2H), 7.38-7.40 (d, J=7.6 Hz, 1H), 7.55-7.61 (m, 3H), 7.80-7.82 (d, J=7.6 Hz, 1H), 7.96-7.98 (d, J=8 Hz, 2H), 8.58 (s, 1H); LC-MS (ESI) m/z: 308 (M+1)+.

후처리

  1. temperatureunder reflux overnight
  2. filtrationThe mixture was filtered
  3. customthe solvent was evaporated under reduced pressure
  4. customthe residue was re-crystallized

출처 및 근거

ORD 기록
ord-b0d00532303843cb954fc61dcf7a6946
출처 데이터셋
uspto-grants-2015_04
특허 번호
US08999987B2

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