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N-bromobutanimide → HCID 59140115, 화합물

HRID 1500696
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HRID 1500696 반응식
[CH3:1][O:2][C:3](=[O:27])[C:4]1[CH:9]=[C:8]([F:10])[C:7]([CH2:11][NH:12][CH:13]=[O:14])=[N:6][C:5]=1[NH:15][C:16]1[CH:21]=[CH:20][C:19]([Si](C)(C)C)=[CH:18][C:17]=1[F:26].C1C(=O)N([Br:35])C(=O)C1>ClCCl>[CH3:1][O:2][C:3](=[O:27])[C:4]1[CH:9]=[C:8]([F:10])[C:7]([CH2:11][NH:12][CH:13]=[O:14])=[N:6][C:5]=1[NH:15][C:16]1[CH:21]=[CH:20][C:19]([Br:35])=[CH:18][C:17]=1[F:26]
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참가 물질

4

반응물 2

HCID 67184N-bromobutanimideHCID 59140138HCID 59140138, 화합물

생성물 1

HCID 59140115HCID 59140115, 화합물수율 95%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
-30 °C

실험 절차

To a solution of 5-fluoro-2-(2-fluoro-4-trimethylsilanyl-phenylamino)-6-formylaminomethyl-nicotinic acid methyl ester (2.6 g, 6.6 mmol) in dichloromethane (65 mL) at −30° C. was added NBS (1.2 g, 6.6 mmol). The reaction mixture was stirred at −30° C. for 1.5 hours, and then concentrated under reduced pressure The resultant residue was taken up in ethyl acetate and this organic solution was washed with a saturated aqueous solution of sodium bicarbonate, followed by brine, dried (Na2SO4), filtered and evaporated in vacuo to afford the title compound as a brown solid (2.49 g, 95%). LCMS (method B): RT=3.79 min, [M+H]+=400/402.

후처리

  1. concentrationconcentrated under reduced pressure The resultant residue
  2. washthis organic solution was washed with a saturated aqueous solution of sodium bicarbonate
  3. dry with materialdried (Na2SO4)
  4. filtrationfiltered
  5. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-d3b9c660e45b494bb8e715aad3bcd668
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09206174B2

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