Toluene → HCID 66990275、化合物

HRID 1697043ノート

反応式

HRID 1697043 の反応式
[C:1]([C:4]1[CH:5]=[CH:6][C:7]([F:15])=[C:8]([N:10]([CH3:14])[C:11](=[O:13])[CH3:12])[CH:9]=1)(=[O:3])[CH3:2].C1(C)C=CC=CC=1>CCCCCCC>[CH3:8][N:10]([CH3:14])[CH:11]=[CH:2][C:1]([C:4]1[CH:5]=[CH:6][C:7]([F:15])=[C:8]([N:10]([CH3:14])[C:11](=[O:13])[CH3:12])[CH:9]=1)=[O:3]

参加物

4

反応物 2

HCID 1140TolueneHCID 46843030N-(5-Acetyl-2-fluorophenyl)-N-methylacetamide

生成物 1

HCID 66990275HCID 66990275、化合物収率 176.8%

試薬・触媒・溶媒 1

HCID 8900Heptane溶媒

反応条件

温度
17.5 °C

実験手順

75.0 g (0.36 moles) of N-(5-acetyl-2-fluorophenyl)-N-methyl-acetamide (VI) were dissolved in 96.3 mL (86.4 g, 0.72 moles) of NNDMF-DMA. The resulting solution was refluxed for 8 hours. At the temperature of 80° C., 400 mL of toluene were added, and then, at the same temperature, 400 mL of n-heptane were slowly added. The resulting solution was slowly cooled to 15-20° C. The white-yellowish solid obtained by recrystallization was filtered off, washed with 263 mL of toluene:n-heptane (1:1), and then dried under vacuum at 40° C. A white-yellowish solid (84.1 g, 91.7% yield) with a melting point=131-132° C. was obtained.

後処理

  1. temperatureThe resulting solution was refluxed for 8 hours
  2. customThe white-yellowish solid obtained by recrystallization
  3. filtrationwas filtered off
  4. washwashed with 263 mL of toluene:n-heptane (1:1)
  5. customdried under vacuum at 40° C

出典と根拠

ORDレコード
ord-99c8def0338b4736802b56a6dbf2b9f5
出典データセット
uspto-grants-2012_04
特許番号
US08163903B2

反応ノート

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