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Ammonium Chloride → 1-Bromo-3-fluoro-5-(methylsulfanyl)benzene

HRID 657512
ノート
印刷プレビュー

反応式

HRID 657512 の反応式
[Br:1][C:2]1[CH:7]=[C:6](F)[CH:5]=[C:4]([F:9])[CH:3]=1.[CH3:10][S-:11].[Na+].[Cl-].[NH4+]>CN(C=O)C>[Br:1][C:2]1[CH:7]=[C:6]([S:11][CH3:10])[CH:5]=[C:4]([F:9])[CH:3]=1
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 3

HCID 25517Ammonium ChlorideHCID 1363131-Bromo-3,5-difluorobenzeneHCID 4378561Sodium methanethiolate

生成物 1

HCID 534144401-Bromo-3-fluoro-5-(methylsulfanyl)benzene収率 84.7%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

50.0 g of 1-bromo-3,5-difluorobenzene and 18.2 g sodium methanethiolate were stirred at 150° C. for 15 min in 300 ml of anhydrous DMF. Subsequently, the mixture was cooled to room temperature, poured onto 1 l of saturated aqueous ammonium chloride solution and extracted three times with 200 ml each of EA. The combined organic phases were dried over magnesium sulfate and the solvent was removed in vacuo. 48.5 g of the title compound were obtained as a pale yellow oil.

後処理

  1. extractionextracted three times with 200 ml each of EA
  2. dry with materialThe combined organic phases were dried over magnesium sulfate
  3. customthe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-0fed665e646b48949a77f488e0853f68
出典データセット
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08076324B2

反応ノート

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