Acetic Acid → HCID 69063437, 화합물

HRID 730431노트

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HRID 730431 반응식
[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

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 109550394-Fluoro-alpha-(4-fluorophenyl)benzenemethanamineHCID 86606793HCID 86606793, 화합물

생성물 1

HCID 69063437HCID 69063437, 화합물

시약·촉매·용매 1

HCID 962Water용매

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온도
100 °C

실험 절차

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%

후처리

  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%

출처 및 근거

ORD 기록
ord-96fc6d4be570439583138995162dc8a3
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07582651B2

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