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Sodium Sulfate → 6-(4-{[3-(7-Methoxy-2-oxoquinoxalin-1(2H)-yl)propyl]amino}-2-oxopyrrolidin-1-yl)-2H-1,4-benzoxazin-3(4H)-one

HRID 1846998
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HRID 1846998 반응식
[NH2:1][CH:2]1[CH2:6][N:5]([C:7]2[CH:8]=[CH:9][C:10]3[O:15][CH2:14][C:13](=[O:16])[NH:12][C:11]=3[CH:17]=2)[C:4](=[O:18])[CH2:3]1.[CH3:19][O:20][C:21]1[CH:30]=[C:29]2[C:24]([N:25]=[CH:26][C:27](=[O:35])[N:28]2[CH2:31][CH2:32][CH:33]=O)=[CH:23][CH:22]=1.S([O-])([O-])(=O)=O.[Na+].[Na+].C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(=O)([O-])O.[Na+]>CN(C)C=O.ClCCl>[CH3:19][O:20][C:21]1[CH:30]=[C:29]2[C:24]([N:25]=[CH:26][C:27](=[O:35])[N:28]2[CH2:31][CH2:32][CH2:33][NH:1][CH:2]2[CH2:6][N:5]([C:7]3[CH:8]=[CH:9][C:10]4[O:15][CH2:14][C:13](=[O:16])[NH:12][C:11]=4[CH:17]=3)[C:4](=[O:18])[CH2:3]2)=[CH:23][CH:22]=1
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참가 물질

8

반응물 5

HCID 24436Sodium SulfateHCID 516892Sodium BicarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 824984066-(4-Amino-2-oxopyrrolidin-1-yl)-2H-1,4-benzoxazin-3(4H)-oneHCID 867249283-(7-Methoxy-2-oxoquinoxalin-1(2H)-yl)propanal

생성물 1

HCID 60141293
6-(4-{[3-(7-Methoxy-2-oxoquinoxalin-1(2H)-yl)propyl]amino}-2-oxopyrrolidin-1-yl)-2H-1,4-benzoxazin-3(4H)-one
수율 97%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매

실험 절차

6-(4-Amino-2-oxopyrrolidin-1-yl)-2H-1,4-benzoxazin-3(4H)-one (Reference Example 6; 106 mg, 0.431 mmol) and 3-(7-methoxy-2-oxoquinoxalin-1(2H)-yl)propanal (100 mg, 0.431 mmol) were dissolved in N,N-dimethylformamide (2 ml), and the mixture to which sodium sulfate (400 mg) was added was stirred overnight at room temperature. The reaction solution was diluted with dichloromethane (12 ml), sodium triacetoxyborohydride (110 mg, 0.517 mmol) was added thereto and the mixture was stirred at room temperature for 3 hours. After completion of the reaction, a saturated sodium hydrogen carbonate aqueous solution was added thereto, the organic layer was separated, washed sequentially with saturated sodium chloride solution, water (×3) and saturated sodium chloride solution, dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure. The obtained residue was purified by silica gel column chromatography (chloroform/methanol) to yield 193 mg (97%) of the title compound in the form of a light brown solid.

후처리

  1. additionwas added
  2. stirringthe mixture was stirred at room temperature for 3 hours
  3. customAfter completion of the reaction
  4. customthe organic layer was separated
  5. washwashed sequentially with saturated sodium chloride solution, water (×3) and saturated sodium chloride solution
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customthe solvent was removed under reduced pressure
  8. customThe obtained residue was purified by silica gel column chromatography (chloroform/methanol)

출처 및 근거

ORD 기록
ord-1db0bb88578b4f43b660f503370cf946
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08952010B2

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