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Bromine → HCID 58085702, 화합물

HRID 249722
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HRID 249722 반응식
[C:1]([C:4]1[CH:5]=[C:6]([NH:16][C:17](=[O:22])[C:18]([F:21])([F:20])[F:19])[CH:7]=[C:8]([S:10]([F:15])([F:14])([F:13])([F:12])[F:11])[CH:9]=1)(=[O:3])[CH3:2].[Br:23]Br>C(O)(=O)C.O>[Br:23][CH2:2][C:1]([C:4]1[CH:5]=[C:6]([NH:16][C:17](=[O:22])[C:18]([F:21])([F:19])[F:20])[CH:7]=[C:8]([S:10]([F:14])([F:15])([F:13])([F:12])[F:11])[CH:9]=1)=[O:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 24408BromineHCID 58085708HCID 58085708, 화합물

생성물 1

HCID 58085702HCID 58085702, 화합물

시약·촉매·용매 2

HCID 176Acetic Acid용매3회HCID 962Water용매

실험 절차

N-(3-Acetyl-5-pentafluorosulfanylphenyl)-2,2,2-trifluoroacetamide (20 mg) was initially introduced dissolved in glacial acetic acid (1 ml), and bromine (9 mg) dissolved in glacial acetic acid (90 μl) was slowly added dropwise. After stirring at RT for 30 min, the mixture was warmed at 60° C. for 1 h. After cooling to RT, the glacial acetic acid was diluted with a large quantity of water and extracted three times with ethyl acetate. The combined extracts were washed with sodium hydrogencarbonate solution until acid-free, dried over magnesium sulfate, filtered and concentrated. The crude product obtained (24 mg) was employed in the next stage without further purification.

후처리

  1. additionwas slowly added dropwise
  2. temperaturethe mixture was warmed at 60° C. for 1 h
  3. temperatureAfter cooling to RT
  4. extractionextracted three times with ethyl acetate
  5. washThe combined extracts were washed with sodium hydrogencarbonate solution until acid-free,
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-efe9cead89d5473296e50d7cb6a79c9b
출처 데이터셋
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07863269B2

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