Acetic Acid → HCID 69063437、化合物

HRID 730431ノート

反応式

HRID 730431 の反応式
[K].[CH:2]([CH:4]([CH2:7][C:8]#[N:9])[C:5]#[N:6])=O.[F:10][C:11]1[CH:16]=[CH:15][C:14]([CH:17]([C:19]2[CH:24]=[CH:23][C:22]([F:25])=[CH:21][CH:20]=2)[NH2:18])=[CH:13][CH:12]=1.C(O)(=O)C>O>[F:10][C:11]1[CH:12]=[CH:13][C:14]([CH:17]([NH:18]/[CH:2]=[C:4](\[CH2:7][C:8]#[N:9])/[C:5]#[N:6])[C:19]2[CH:24]=[CH:23][C:22]([F:25])=[CH:21][CH:20]=2)=[CH:15][CH:16]=1

参加物

5

反応物 3

HCID 176Acetic AcidHCID 109550394-Fluoro-alpha-(4-fluorophenyl)benzenemethanamineHCID 86606793HCID 86606793、化合物

生成物 1

HCID 69063437HCID 69063437、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

To a solution of formyl succinonitrile potassium salt (6.67 g, 45.6 mmol) and 1,1-bis(4-fluorophenyl) methaneamine (11.0 g, 50.2 mmol) in water (19 ml) was added acetic acid (19 ml) at room temperature, and the mixture was stirred 100° C. for 30 minutes. The solvent was distilled off under reduced pressure. The residue was poured into iced water, made basic with potassium carbonate and then extracted with ethyl acetate. The extract was washed with water and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure to give the objective product as oily matter. Yield (amount) 14.0 g, yield (rate) 99.3%

後処理

  1. distillationThe solvent was distilled off under reduced pressure
  2. additionThe residue was poured into iced water
  3. extractionextracted with ethyl acetate
  4. washThe extract was washed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. customto give the objective product as oily matter
  8. customYield (amount) 14.0 g
  9. customyield (rate) 99.3%

出典と根拠

ORDレコード
ord-96fc6d4be570439583138995162dc8a3
出典データセット
uspto-grants-2009_09
特許番号
US07582651B2

反応ノート

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