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Cyanogen Bromide → HCID 58045867, 화합물

HRID 657855
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인쇄 미리보기

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HRID 657855 반응식
[N:1]1([C:6]2[N:11]=[N:10][C:9]([NH:12][NH2:13])=[CH:8][CH:7]=2)[CH:5]=[CH:4][N:3]=[CH:2]1.C([O-])(=O)C.[Na+].[N:19]#[C:20]Br.[OH-].[Na+]>C(O)(=O)C.O>[N:1]1([C:6]2[CH:7]=[CH:8][C:9]3[N:10]([C:20]([NH2:19])=[N:13][N:12]=3)[N:11]=2)[CH:5]=[CH:4][N:3]=[CH:2]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 10476Cyanogen BromideHCID 14798Sodium HydroxideHCID 517045Sodium AcetateHCID 30313233-hydrazinyl-6-(1H-imidazol-1-yl)pyridazine

생성물 1

HCID 58045867HCID 58045867, 화합물수율 11.6%

시약·촉매·용매 2

HCID 176Acetic Acid용매
HCID 962
Water
용매

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온도
0 °C

실험 절차

(6-Imidazol-1-ylpyridazin-3-yl)hydrazine (500 mg) were initially charged in a mixture of acetic acid (4 ml) and water (8 ml) with addition of sodium acetate (232 mg) at RT while stirring. Thereafter, the mixture was cooled to 0° C. and cyanogen bromide (330 mg) was introduced in portions. After stirring for 2.5 h, the mixture was left to stand overnight. After cooling to 0° C., the mixture was alkalized with 10 M sodium hydroxide solution and extracted repeatedly with EA. The combined EA phases were dried over sodium sulfate, filtered and concentrated. 66 mg of the title compound were isolated.

후처리

  1. stirringAfter stirring for 2.5 h
  2. waitthe mixture was left
  3. temperatureAfter cooling to 0° C.
  4. extractionextracted repeatedly with EA
  5. dry with materialThe combined EA phases were dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-5a036a86ac02487da2fa37c559008312
출처 데이터셋
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08076336B2

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