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4-Bromoaniline → HCID 531936, 화합물

HRID 897996
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HRID 897996 반응식
[F:1][C:2]1[CH:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4](Cl)=[O:5].[Br:11][C:12]1[CH:18]=[CH:17][C:15]([NH2:16])=[CH:14][CH:13]=1.C(N(CC)C(C)C)(C)C>ClCCl>[Br:11][C:12]1[CH:18]=[CH:17][C:15]([NH:16][C:4](=[O:5])[C:3]2[CH:7]=[CH:8][CH:9]=[CH:10][C:2]=2[F:1])=[CH:14][CH:13]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 78074-BromoanilineHCID 98082-Fluorobenzoyl chlorideHCID 81531Diisopropylethylamine

생성물 1

HCID 531936HCID 531936, 화합물수율 88.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 2-fluorobenzoyl chloride (5.82 g, 0.0367 mol) and 4-bromoaniline (6.31 g, 0.0367 mol) in anhydrous dichloromethane (150 mL) was cooled to 0° C. and N,N-diisopropylethylamine (5.21 g, 0.0407 mol) was added under nitrogen atmosphere dropwise. The resulting mixture was stirred at ambient temperature for 24 hours, concentrated and the residue partitioned between ethyl acetate (120 mL) and water (100 mL). The organic phase was washed with brine, dried with magnesium sulfate and concentrated. The residue was suspended in cold diethyl ether (50 mL) and the precipitate was collected by filtration and dried to yield N1-(4-bromophenyl)-2-fluorobenzamide (9.6 g, 0.0326 mol) as a white solid.

후처리

  1. concentrationconcentrated
  2. customthe residue partitioned between ethyl acetate (120 mL) and water (100 mL)
  3. washThe organic phase was washed with brine
  4. dry with materialdried with magnesium sulfate
  5. concentrationconcentrated
  6. filtrationthe precipitate was collected by filtration
  7. customdried

출처 및 근거

ORD 기록
ord-c8f252f6b30549d48358b52d06d2deaa
출처 데이터셋
uspto-grants-2005_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06921763B2

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