4-Methylmorpholine → HCID 67050039, 화합물

HRID 217631

반응식

HRID 217631 반응식
CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[NH2:25][C:26]1[C:30]([NH:31][C:32]([O:34][C:35]([CH3:38])([CH3:37])[CH3:36])=[O:33])=[CH:29][S:28][CH:27]=1.[CH3:39][O:40][C:41]([C:43]1[CH:44]=[CH:45][C:46]([C:49](O)=[O:50])=[N:47][CH:48]=1)=[O:42].CN1CCOCC1>CN(C=O)C.C(OCC)(=O)C.O>[C:35]([O:34][C:32]([NH:31][C:30]1[C:26]([NH:25][C:49]([C:46]2[CH:45]=[CH:44][C:43]([C:41]([O:40][CH3:39])=[O:42])=[CH:48][N:47]=2)=[O:50])=[CH:27][S:28][CH:29]=1)=[O:33])([CH3:38])([CH3:37])[CH3:36]

참가 물질

8

반응물 4

HCID 79724-MethylmorpholineHCID 3149925-(Methoxycarbonyl)pyridine-2-carboxylic acidHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 11063797HCID 11063797, 화합물

생성물 1

HCID 67050039HCID 67050039, 화합물수율 67%

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

HATU (1.3 g, 3.5 mmol) was added to a solution of 3-amino-4-t-butoxycarbonylaminothiophene (Reference Compound No. 1-1, 0.68 g, 3.2 mmol), 5-methoxycarbonylpyridine-2-carboxylic acid (0.64 g, 3.5 mmol), and N-methylmorpholine (0.70 mL, 6.4 mmol) in DMF (20 mL), and then the reaction mixture was stirred at room temperature overnight. Water (0.30 L) and ethyl acetate (0.40 L) were added thereto, and the insoluble materials were filtered off to give 0.50 g of the title reference compound as a pale yellow solid. The filtrate was partitioned and the organic layer was dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and then the obtained solid was collected by filtration with ethylacetate (30 mL) to give 0.30 g of the title reference compound as a pale brown solid. (Yield 67%)

후처리

  1. filtrationthe insoluble materials were filtered off
  2. customto give 0.50 g of the title reference compound as a pale yellow solid
  3. customThe filtrate was partitioned
  4. dry with materialthe organic layer was dried over anhydrous sodium sulfate
  5. customThe solvent was evaporated under reduced pressure
  6. filtrationthe obtained solid was collected by filtration with ethylacetate (30 mL)
  7. customto give 0.30 g of the title reference compound as a pale brown solid

출처 및 근거

ORD 기록
ord-10d61d39493341c88cd84f7b81bfdad3
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08198271B2

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