5-Fluoro-2-methylthiophenol → HCID 21162454、化合物

HRID 894250ノート

反応式

HRID 894250 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[SH:9].Br[C:11]1[O:15][CH:14]=[C:13]([C:16]([OH:18])=[O:17])[CH:12]=1>CN(C)C=O>[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[S:9][C:11]1[O:15][CH:14]=[C:13]([C:16]([OH:18])=[O:17])[CH:12]=1

参加物

4

反応物 2

HCID 27590435-Fluoro-2-methylthiophenolHCID 133335605-Bromofuran-3-carboxylic acid

生成物 1

HCID 21162454HCID 21162454、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

In an open flask cuprous oxide (500 mg., 3.5 mmoles) and 2-methyl-5-fluorothiophenol (1.0 g., 7 mmoles) were combined in 35 ml. of dimethylformamide and heated in an oil bath at 135°-140° C. for 2.5 hours. The mixture was cooled slightly, 5-bromofuran-3-carboxylic acid (668 mg., 3.5 mmoles) was added and the mixture refluxed for approximately 16 hours. Crude product was isolated according to Example 16. The resulting oil was crystallized by trituration with water (170 mg.). Recrystallization from methanol/water gave purified 5-(2-methyl-5-fluorophenylthio)furan-3-carboxylic acid (125 mg., m.p. 150°-152° C., m/e 252).

後処理

  1. temperatureThe mixture was cooled slightly
  2. temperaturethe mixture refluxed for approximately 16 hours
  3. customCrude product was isolated
  4. customThe resulting oil was crystallized by trituration with water (170 mg.)
  5. customRecrystallization from methanol/water
  6. customgave
  7. custompurified 5-(2-methyl-5-fluorophenylthio)furan-3-carboxylic acid (125 mg., m.p. 150°-152° C., m/e 252)

出典と根拠

ORDレコード
ord-df7ecbdbd59240b8a666daea32310ceb
出典データセット
uspto-grants-1981_08
特許番号
US04282246

反応ノート

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