Potassium Carbonate → HCID 58098809, 화합물

HRID 384261

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HRID 384261 반응식
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[NH:11][C:12](=[O:14])[CH3:13].[H-].[Na+].C([O-])([O-])=O.[K+].[K+].Cl.Cl[CH2:25][CH2:26][N:27]1[CH2:31][CH2:30][CH2:29][CH2:28]1>CN(C=O)C>[N+:8]([C:5]1[CH:6]=[CH:7][C:2]([O:1][CH2:25][CH2:26][N:27]2[CH2:31][CH2:30][CH2:29][CH2:28]2)=[C:3]([NH:11][C:12](=[O:14])[CH3:13])[CH:4]=1)([O-:10])=[O:9]

참가 물질

6

반응물 4

HCID 11430Potassium CarbonateHCID 24758Sodium hydrideHCID 816681-(2-Chloroethyl)pyrrolidine hydrochlorideHCID 3292867Acetamide, N-(2-hydroxy-5-nitrophenyl)-

생성물 1

HCID 58098809HCID 58098809, 화합물수율 33%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
100 °C

실험 절차

To a solution of N-(2-hydroxy-5-nitrophenyl)acetamide (870 mg, 4.44 mmol) in DMF (5 mL) was added NaH (196 mg, 5.32 mmol) and K2CO3 (2.11 g, 13.32 mmol), followed by 1-(2-chloroethyl)pyrrolidine hydrochloride (905 mg, 5.32 mmol). After heating at 100° C. for 20 h, the solution was poured to ice, and was extracted with EtOAc, organic layer was washed with Sat. NaHCO3, brine, dried and concentrated to give N-(5-nitro-2-(2-(pyrrolidin-1-yl)ethoxy)phenyl)acetamide (430 mg).

후처리

  1. additionthe solution was poured to ice
  2. extractionwas extracted with EtOAc, organic layer
  3. washwas washed with Sat. NaHCO3, brine
  4. customdried
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-182f0f1697c64ecc978d4050f6b5f349
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08367689B2

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