Trifluoroacetic acid → HCID 86729754、化合物

HRID 2272595ノート

反応式

HRID 2272595 の反応式
[C:1]([C:3]1[CH:23]=[CH:22][C:6]([C:7]([NH:9][CH2:10][CH:11]([CH3:21])[CH2:12][NH:13]C(=O)OC(C)(C)C)=[O:8])=[CH:5][CH:4]=1)#[N:2].C(O)(C(F)(F)F)=O>>[NH2:13][CH2:12][CH:11]([CH3:21])[CH2:10][NH:9][C:7](=[O:8])[C:6]1[CH:22]=[CH:23][C:3]([C:1]#[N:2])=[CH:4][CH:5]=1

参加物

3

反応物 2

HCID 6422Trifluoroacetic acidHCID 86729753HCID 86729753、化合物

生成物 1

HCID 86729754HCID 86729754、化合物収率 93%

実験手順

A solution of the compound obtained in Step 1 (311 mg, 0.98 mmol) in TFA (1 mL, 12.98 mmol) was stirred at room temperature for 15 min, and concentrated under reduced pressure. To the residue were added ethyl acetate and 1N aqueous sodium hydroxide solution, and the organic layer was separated. The organic layer was washed with water and saturated brine, and dried, and the solvent was evaporated under reduced pressure to give N-(3-amino-2-methylpropyl)-4-cyanobenzamide (198 mg, 0.911 mmol, 93%) as a white powder.

後処理

  1. concentrationconcentrated under reduced pressure
  2. additionTo the residue were added ethyl acetate and 1N aqueous sodium hydroxide solution
  3. customthe organic layer was separated
  4. washThe organic layer was washed with water and saturated brine
  5. customdried
  6. customthe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-ea71da72c2ae484894e00a9812b9d64f
出典データセット
uspto-grants-2015_09
特許番号
US09120776B2

反応ノート

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