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Water → HCID 1019799, 화합물

HRID 2041800
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HRID 2041800 반응식
[Br:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([CH:10]=1)[C:7](Cl)=[O:8].[Br:11][C:12]1[CH:18]=[CH:17][CH:16]=[CH:15][C:13]=1[NH2:14].C(N(CC)CC)C.O>ClCCl>[Br:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([CH:10]=1)[C:7]([NH:14][C:13]1[CH:15]=[CH:16][CH:17]=[CH:18][C:12]=1[Br:11])=[O:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 119922-BromoanilineHCID 27812235-Bromonicotinoyl chloride

생성물 1

HCID 1019799HCID 1019799, 화합물수율 85.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of 5-bromonicotinoyl chloride (3) (7.5 g, 33 mmol), 2-bromoaniline (5.86 g, 33 mmol) and triethylamine (NEt3) (14 mL, 100 mmol) in anhydrous dichlormethane (DCM) (100 mL) was stirred under argon overnight. The resulting mixture was worked up with water and extracted with dichloromethane (200 mL×2). The organic phase was collected and dried over Na2SO4. After concentrating to 150 mL, a white crystalline solid was crashed precipitated out. Filtration and washing with hexanes gave a white solid 4 (10.0 g, 85% yield).

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후처리

  1. extractionextracted with dichloromethane (200 mL×2)
  2. customThe organic phase was collected
  3. dry with materialdried over Na2SO4
  4. concentrationAfter concentrating to 150 mL
  5. customa white crystalline solid was crashed precipitated out
  6. filtrationFiltration
  7. washwashing with hexanes

출처 및 근거

ORD 기록
ord-6b5a1ad25a264b4f907ca04c51124895
출처 데이터셋
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08585926B2

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