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Water → HCID 58792696, 화합물

HRID 1365089
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HRID 1365089 반응식
Cl[CH2:2][C:3]([NH:5][C:6]1[CH:7]=[CH:8][C:9]2[C:10](=[O:19])[C:11]3[C:16]([C:17]=2[CH:18]=1)=[CH:15][CH:14]=[CH:13][CH:12]=3)=[O:4].C([O-])([O-])=O.[K+].[K+].O.[C:27]([O:30][CH2:31]C)(=[O:29])[CH3:28].C[N:34]([CH:36]=O)[CH3:35]>>[CH3:31][O:30][C:27](=[O:29])[C:28]1[CH:17]=[CH:9][CH:8]=[CH:7][C:36]=1[NH:34][CH:35]1[CH2:18][CH2:6][N:5]([CH2:2][C:3](=[O:4])[NH:5][C:6]2[CH:7]=[CH:8][C:9]3[C:10](=[O:19])[C:11]4[C:16]([C:17]=3[CH:18]=2)=[CH:15][CH:14]=[CH:13][CH:12]=4)[CH2:3][CH2:2]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 5

HCID 962WaterHCID 6228DimethylformamideHCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 114486452-Chloro-N-(9-oxo-9H-fluoren-3-yl)-acetamide

생성물 1

HCID 58792696HCID 58792696, 화합물수율 77%

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온도
10 °C

실험 절차

A mixture of 2-(Piperidine-4-yl-amino)-methyl benzoate (1100 mg, 4.70 mmol), 2-Chloro-N-(9-oxo-9H-fluoren-3-yl)-acetamide (1358 mg, 5 mmol) and K2CO3 (1380 mg, 10 mmol) in DMF (40 mL) was stirred at 10° C. for 2 hours and then at room temperature overnight. The reaction mixture was added to 50 mL water and 100 mL ethyl acetate, the organic phase was decanted and washed with water (3×50 mL), dried over sodium sulfate and a 2.8 M hydrogen chloride solution in absolute ethanol (1.80 mL) was added, to precipitate the hydrochloride, which was filtered off and washed with ethyl acetate. 1840 mg of a white solid were obtained. Yield: 77%.

후처리

  1. customat room temperature
  2. customovernight
  3. customthe organic phase was decanted
  4. washwashed with water (3×50 mL)
  5. dry with materialdried over sodium sulfate
  6. additiona 2.8 M hydrogen chloride solution in absolute ethanol (1.80 mL) was added
  7. customto precipitate the hydrochloride, which
  8. filtrationwas filtered off
  9. washwashed with ethyl acetate

출처 및 근거

ORD 기록
ord-de5906374a9d403e8d8892522d3b5894
출처 데이터셋
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07888510B2

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