Trifluoroacetic acid → 4-(2-Aminoethyl)benzonitrile

HRID 44419ノート

反応式

HRID 44419 の反応式
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH2:10][NH:11]C(=O)OC(C)(C)C)=[CH:5][CH:4]=1)#[N:2].C(O)(C(F)(F)F)=O>C(Cl)Cl>[C:1]([C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH2:10][NH2:11])=[CH:5][CH:4]=1)#[N:2]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 21955533tert-Butyl 4-cyanophenethylcarbamate

生成物 1

HCID 219125254-(2-Aminoethyl)benzonitrile収率 95.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Compound 114 (308 mg, 1.25 mmol) was dissolved in DCM (4 mL) and the solution was cooled in an ice-water bath. TFA (3.5 mL) was then added and the mixture was stirred at room temperature for 15 min. The reaction mixture was concentrated in vacuo and the residue was dissolved in EtOAc (50 mL). The solution was washed with K2CO3 (sat., 3×), brine, dried and concentrated to yield 115 (175 mg, 95%) as a pale yellow oil. MS (APCI): m/z 147 [M+H]+.

後処理

  1. temperaturethe solution was cooled in an ice-water bath
  2. concentrationThe reaction mixture was concentrated in vacuo
  3. dissolutionthe residue was dissolved in EtOAc (50 mL)
  4. washThe solution was washed with K2CO3 (sat., 3×), brine
  5. customdried
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-a766666a5cee47efaed4399655e05a4c
出典データセット
uspto-grants-2013_09
特許番号
US08541423B2

反応ノート

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