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Water → HCID 21931732, 화합물

HRID 2209283
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HRID 2209283 반응식
[Cl:1][C:2]1[N:7]=C2N[C:9](=O)[CH2:10][C:5]2=[CH:4][CH:3]=1.[H-].[Na+].I[CH3:15].O.[CH3:17][N:18]([CH:20]=[O:21])[CH3:19]>[Cl-].[Na+].O.CCOC(C)=O>[Cl:1][C:2]1[N:7]=[C:17]2[N:18]([CH3:19])[C:20](=[O:21])[C:10]([CH3:9])([CH3:15])[C:5]2=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 962WaterHCID 6228Dimethylformamide2회HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 219070476-Chloro-1,3-dihydro-2H-pyrrolo[2,3-b]pyridin-2-one

생성물 1

HCID 21931732HCID 21931732, 화합물

시약·촉매·용매 2

HCID 8857
Ethyl Acetate
용매
HCID 57417360Sodium chloride; water용매

실험 절차

To a solution of 6-chloro-1H-pyrrolo[2,3-b]pyridin-2(3H)-one (50 mg, 0.30 mmol) in DMF (1 mL) at 0° C. was added NaH (48 mg, 1.2 mmol, 60%), and the reaction was stirred for 5 minutes. Iodomethane (210 mg, 1.5 mmol) was added and the reaction became a thick slurry. DMF (0.5 mL) was added and the reaction was stirred at room temperature for 90 minutes. Water, EtOAc, and brine were added, the layers were separated and the organic layer was washed with brine. The organics were dried over MgSO4, filtered and concentrated to afford 6-chloro-1,3,3-trimethyl-1H-pyrrolo[2,3-b]pyridin-2(3H)-one 7.28 which was used without further purification. LCMS-ESI+ (m/z): [M+H]+ calcd for C10H12ClN2O: 211.1; found: 211.0.

후처리

  1. stirringthe reaction was stirred at room temperature for 90 minutes
  2. customthe layers were separated
  3. washthe organic layer was washed with brine
  4. dry with materialThe organics were dried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-c88d4d85d3904d1086c79f9e11e9607f
출처 데이터셋
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09376441B2

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