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Methanol → 4-Amino-5-fluoro-2-methoxybenzonitrile

HRID 630409
ノート
印刷プレビュー

反応式

HRID 630409 の反応式
[CH3:1][OH:2].[NH2:3][C:4]1[C:11]([F:12])=[CH:10][C:7]([C:8]#[N:9])=[C:6](F)[CH:5]=1>O1CCCC1>[NH2:3][C:4]1[C:11]([F:12])=[CH:10][C:7]([C:8]#[N:9])=[C:6]([O:2][CH3:1])[CH:5]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 887MethanolHCID 27359004-Amino-2,5-difluorobenzonitrile

生成物 1

HCID 185196344-Amino-5-fluoro-2-methoxybenzonitrile収率 97%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a mixture of methanol (10.48 mL, 0.25 mol) and anh. tetrahydrofuran (60 mL) was added dropwise a solution of potassium tert-butilate (6.76 g, 0.05 mol) in anh. tetrahydrofuran (52 mL) at 0° C. under nitrogen atmosphere. The mixture was stirred for minutes at room temperature and then 4-amino-2,5-difluorobenzonitrile (4 g, 0.02 mol) was added. The reaction mixture was stirred at 70° C. for 3 hours. The solvent was partially removed and ether was added into the mixture. The organic layer was washed with bicarbonate and brine, dried and filtered. The organic solvent was removed under reduced pressure to give the title compound as a yellow solid (97%), which was used in the next step without further purification.

後処理

  1. stirringThe reaction mixture was stirred at 70° C. for 3 hours
  2. customThe solvent was partially removed
  3. additionether was added into the mixture
  4. washThe organic layer was washed with bicarbonate and brine
  5. customdried
  6. filtrationfiltered
  7. customThe organic solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-8242f9408a2247d490ba5d83aed76b62
出典データセット
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09315463B2

反応ノート

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