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Bromine → HCID 58085702、化合物

HRID 249722
ノート
印刷プレビュー

反応式

HRID 249722 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 24408BromineHCID 58085708HCID 58085708、化合物

生成物 1

HCID 58085702HCID 58085702、化合物

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒3 回HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-efe9cead89d5473296e50d7cb6a79c9b
出典データセット
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07863269B2

反応ノート

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