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Tetrafluoroboric acid → 5-Bromo-2,4-difluoro-3-methylbenzenediazonium tetrafluoroborate

HRID 330075
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HRID 330075 반응식
[Br:1][C:2]1[C:3]([F:11])=[C:4]([CH3:10])[C:5]([F:9])=[C:6]([CH:8]=1)[NH2:7].[N:12]([O-])=O.[Na+].[F:16][B-:17]([F:20])([F:19])[F:18].[H+]>O>[F:16][B-:17]([F:20])([F:19])[F:18].[Br:1][C:2]1[C:3]([F:11])=[C:4]([CH3:10])[C:5]([F:9])=[C:6]([N+:7]#[N:12])[CH:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 28118Tetrafluoroboric acidHCID 140525645-Bromo-2,4-difluoro-3-methylbenzenamineHCID 23668193Sodium Nitrite

생성물 1

HCID 140525655-Bromo-2,4-difluoro-3-methylbenzenediazonium tetrafluoroborate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a suspension of 5-bromo-2,4-difluoro-3-methylaniline (24.60 g) in 42% fluoroboric acid (150 ml) with stirring vigorously at -3° to 0° C. was added sodium nitrite (11.47 g) in water (20 ml) dropwise during 40 minutes. After stirring for 1.5 hours at 0° to 5° C., the reacting mixture was cooled with ice bath sufficiently and the resulting precipitate was collected by filtration. This precipitate was washed with small portion of water and ether and dried under reduced pressure to give the title compound (28.83 g) as pale brown prisms, mp 147°-150° C. (decompd.).

후처리

  1. stirringAfter stirring for 1.5 hours at 0° to 5° C.
  2. temperaturethe reacting mixture was cooled with ice bath sufficiently
  3. filtrationthe resulting precipitate was collected by filtration
  4. washThis precipitate was washed with small portion of water and ether
  5. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-95d70f47181146238fd762f7ff864139
출처 데이터셋
uspto-grants-1990_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04894458

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