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Water → HCID 59295129, 화합물

HRID 2233034
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HRID 2233034 반응식
[Cl:1][C:2]1[C:3]([NH:8][NH:9][C:10](=[O:15])[C:11]([F:14])([F:13])[F:12])=[N:4][CH:5]=[CH:6][N:7]=1.N1C=CC=CC=1.[Br:22]Br.O>CC(O)=O>[Br:22][C:6]1[N:7]=[C:2]([Cl:1])[C:3]([NH:8][NH:9][C:10](=[O:15])[C:11]([F:12])([F:13])[F:14])=[N:4][CH:5]=1
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참가 물질

6

반응물 4

HCID 962WaterHCID 1049PyridineHCID 24408BromineHCID 58446973HCID 58446973, 화합물

생성물 1

HCID 59295129HCID 59295129, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

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온도
0 °C

실험 절차

A solution of 2.40 g of the product of Step A and 1.97 g of pyridine in AcOH (10.0 mL) at 0° C. was stirred as a solution of 1.92 g of bromine in AcOH (1.0 mL) was added dropwise. The resulting mixture was stirred at 0° C. for one h and then warmed to ambient temperature and stirred for an additional 16 h. The reaction mixture was poured into water and extracted with EtOAc (2×). The combined organic extracts were washed with water, dried over magnesium sulfate, filtered, and concentrated to an oil that was purified by silica gel chromatography to provide trifluoroacetic acid N′-(5-bromo-3-chloro-pyrazin-2-yl)-hydrazide as a white solid. MS (M+H+)=320.1.

후처리

  1. additionwas added dropwise
  2. temperaturewarmed to ambient temperature
  3. stirringstirred for an additional 16 h
  4. extractionextracted with EtOAc (2×)
  5. washThe combined organic extracts were washed with water
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated to an oil that
  9. customwas purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-7c40a0dece594b1b8479acefcc7612d6
출처 데이터셋
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07709473B2

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