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Hydrogen Bromide → 1-(2-fluoro-4-hydroxyphenyl)-1,4-dihydro-4-(3-fluoropropyl)-5H-tetrazol-5-one

HRID 482402
ノート
印刷プレビュー

反応式

HRID 482402 の反応式
FC1C=CC(C[O:9][C:10]2[CH:15]=[CH:14][C:13]([N:16]3[C:20](=[O:21])[N:19]([CH2:22][CH2:23][CH2:24][F:25])[N:18]=[N:17]3)=[C:12]([F:26])[CH:11]=2)=CC=1.Br>C(O)(=O)C>[F:26][C:12]1[CH:11]=[C:10]([OH:9])[CH:15]=[CH:14][C:13]=1[N:16]1[C:20](=[O:21])[N:19]([CH2:22][CH2:23][CH2:24][F:25])[N:18]=[N:17]1
参加物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 260Hydrogen BromideHCID 189810431-[4-(4-fluorophenylmethoxy)-2-fluorophenyl]-1,4-dihydro-4-(3-fluoropropyl)-5H-tetrazol-5-one

生成物 1

HCID 189810471-(2-fluoro-4-hydroxyphenyl)-1,4-dihydro-4-(3-fluoropropyl)-5H-tetrazol-5-one収率 111%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

To a solution of 5.60 g (0.0153 mole) of 1-[4-(4-fluorophenylmethoxy)-2-fluorophenyl]-1,4-dihydro-4-(3-fluoropropyl)-5H-tetrazol-5-one in 60 mL of glacial acetic acid was added 5 mL of 49% hydrobromic acid. This mixture was heated at reflux for 90 minutes, after which it was cooled to room temperature. The reaction mixture was then poured over ice, and the resulting aqueous solution was extracted with diethyl ether. The combined extract was dried over magnesium sulfate, filtered, and the solvent was evaporated under reduced pressure, leaving 4.35 g of 1-(2-fluoro-4-hydroxy-phenyl)-1,4-dihydro-4-(3-fluoropropyl)-5H-tetrazol-5-one as a residue.

後処理

  1. temperatureThis mixture was heated
  2. temperatureat reflux for 90 minutes
  3. additionThe reaction mixture was then poured over ice
  4. extractionthe resulting aqueous solution was extracted with diethyl ether
  5. extractionThe combined extract
  6. dry with materialwas dried over magnesium sulfate
  7. filtrationfiltered
  8. customthe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-4117a6207fa64e4f80c6e8a865350241
出典データセット
uspto-grants-1998_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05798316

反応ノート

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