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Boron trifluoride etherate → Ethyl 4-Amino-2-fluorobenzoate

HRID 1389071
ノート
印刷プレビュー

反応式

HRID 1389071 の反応式
C([NH:4][C:5]1[CH:13]=[CH:12][C:8]([C:9]([OH:11])=[O:10])=[C:7]([F:14])[CH:6]=1)(=O)C.B(F)(F)F.[CH3:19][CH2:20]OCC>C(O)C>[NH2:4][C:5]1[CH:13]=[CH:12][C:8]([C:9]([O:11][CH2:19][CH3:20])=[O:10])=[C:7]([F:14])[CH:6]=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 8000Boron trifluoride etherateHCID 130413704-Acetamido-2-fluorobenzoic acid

生成物 1

HCID 10797532Ethyl 4-Amino-2-fluorobenzoate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 10.0 g of 4-acetamido-2-fluorobenzoic acid, 100 ml of ethyl alcohol and 2.0 ml of boron trifluoride etherate is heated under reflux for 22 hours. The solvent is slowly removed by distillation as an equal amount of fresh ethyl alcohol is added. After 200 ml of solvent has been removed, the remainder is evaporated at reduced pressure. The residue is dissolved in ethyl acetate, washed with saturated aqueous sodium bicarbonate, dried and the solvent then evaporated to yield a solid. Recrystallization of the solid from ethanol-hexane yields ethyl 4-amino-2-fluorobenzoate.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. temperatureunder reflux for 22 hours
  2. customThe solvent is slowly removed by distillation as an equal amount of fresh ethyl alcohol
  3. additionis added
  4. customAfter 200 ml of solvent has been removed
  5. customthe remainder is evaporated at reduced pressure
  6. dissolutionThe residue is dissolved in ethyl acetate
  7. washwashed with saturated aqueous sodium bicarbonate
  8. customdried
  9. customthe solvent then evaporated
  10. customto yield a solid
  11. customRecrystallization of the solid from ethanol-hexane

出典と根拠

ORDレコード
ord-73fd72f6eca548d3853a6f9fd11893fe
出典データセット
uspto-grants-1981_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04243609

反応ノート

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