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N-bromobutanimide → HCID 17972674, 화합물

HRID 1372533
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HRID 1372533 반응식
[C:1]([NH:4][C:5]1[CH:6]=[C:7]2[C:11](=[CH:12][CH:13]=1)[C:10](=[O:14])[CH:9]([CH2:15][CH3:16])[CH2:8]2)(=[O:3])[CH3:2].[Br:17]N1C(=O)CCC1=O>CN(C)C=O>[C:1]([NH:4][C:5]1[C:6]([Br:17])=[C:7]2[C:11](=[CH:12][CH:13]=1)[C:10](=[O:14])[CH:9]([CH2:15][CH3:16])[CH2:8]2)(=[O:3])[CH3:2]
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참가 물질

4

반응물 2

HCID 67184N-bromobutanimideHCID 202319645-(Acetylamino)-2-ethyl-1-indanone

생성물 1

HCID 17972674HCID 17972674, 화합물수율 93.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
60 °C

실험 절차

A solution of 5-(acetylamino)-2-ethyl-1-indanone (2.32 g, 10.7 mmol) in anhydrous N,N-dimethylformamide (10.7 mL) was treated with N-bromosuccinimide (2.00 g, 11.21 mmol). The mixture was placed under a N2 atmosphere, stirred, and heated in an oil bath at 60° C. for 100 minutes. After cooling to room temperature, the mixture was partitioned between EtOAc (200 mL) and water (200 mL). The organic phase was washed with water (4×200 mL) and brine (100 mL), dried over MgSO4, filtered, and evaporated under vacuum to afford crude 5-(acetylamino)-4-bromo-2-ethyl-1-indanone as a yellow solid (2.95 g).

후처리

  1. temperatureAfter cooling to room temperature
  2. customthe mixture was partitioned between EtOAc (200 mL) and water (200 mL)
  3. washThe organic phase was washed with water (4×200 mL) and brine (100 mL)
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customevaporated under vacuum

출처 및 근거

ORD 기록
ord-99f2b0b026594200a67e1fd0b3be6da9
출처 데이터셋
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07157604B2

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