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Sulfuric Acid → 1-[3-Amino-5-(pentafluorosulfanyl)phenyl]ethanone

HRID 657997
ノート
印刷プレビュー

反応式

HRID 657997 の反応式
[C:1]([C:4]1[CH:5]=[C:6]([NH:16]C(=O)C(F)(F)F)[CH:7]=[C:8]([S:10]([F:15])([F:14])([F:13])([F:12])[F:11])[CH:9]=1)(=[O:3])[CH3:2].S(=O)(=O)(O)O>C(Cl)Cl>[NH2:16][C:6]1[CH:5]=[C:4]([C:1](=[O:3])[CH3:2])[CH:9]=[C:8]([S:10]([F:15])([F:11])([F:12])([F:13])[F:14])[CH:7]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 1118Sulfuric AcidHCID 58085708HCID 58085708、化合物

生成物 1

HCID 581368521-[3-Amino-5-(pentafluorosulfanyl)phenyl]ethanone収率 92.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
100 °C

実験手順

N-(3-Acetyl-5-pentafluorosulfanylphenyl)-2,2,2-trifluoroacetamide (O3.075; 9.4 g) was admixed with semiconcentrated sulfuric acid (200 ml), and DCM (15 ml) was added. After stirring at 100° C. for 7 h, the mixture was left to stand overnight. Then the mixture was added to ice-water and extracted with EA. The combined EA phases were washed with saturated sodium hydrogencarbonate solution, dried over magnesium sulfate, filtered and concentrated by rotary evaporation. 6.36 g of the title compound were obtained. LC-MS rt: 1.38 min [M+H]+: 262.0 (met. a)

後処理

  1. additionwas added
  2. waitthe mixture was left
  3. waitto stand overnight
  4. extractionextracted with EA
  5. washThe combined EA phases were washed with saturated sodium hydrogencarbonate solution
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated by rotary evaporation

出典と根拠

ORDレコード
ord-bf6ee0b1fe7a4117aa0414855fe4187b
出典データセット
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08076336B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート