Aluminium lithium hydride → 3-(Aminomethyl)-2,6-dichloro-5-fluoroaniline

HRID 450331노트

반응식

HRID 450331 반응식
[Cl:1][C:2]1[C:10]([NH2:11])=[C:9]([Cl:12])[C:8]([F:13])=[CH:7][C:3]=1[C:4]([NH2:6])=O.[H-].[H-].[H-].[H-].[Li+].[Al+3]>C1COCC1>[NH2:11][C:10]1[C:2]([Cl:1])=[C:3]([CH:7]=[C:8]([F:13])[C:9]=1[Cl:12])[CH2:4][NH2:6]

참가 물질

4

반응물 2

HCID 21226445Aluminium lithium hydrideHCID 866744963-Amino-2,4-dichloro-5-fluorobenzamide

생성물 1

HCID 825077343-(Aminomethyl)-2,6-dichloro-5-fluoroaniline

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

2,4-Dichloro-5-fluoro-3 amino-benzamide (6.00 g, 26.9 mmol) in THF (175 mL) is added dropwise to LiAlH4 (1 M in THF, 28.0 mL) in THF (175 mL). The reaction mixture is stirred for 1 h at rt and 5 h at reflux. Excess LiAlH4 is destroyed under cooling as described by L. F. Fieser & M. Fieser Vol 1, p 584 Wiley 1967. After 30 min the mixture is filtered, the filtrate is concentrated, diluted with Et2O and the precipitate is collected.

후처리

  1. temperatureat reflux
  2. customExcess LiAlH4 is destroyed
  3. temperatureunder cooling
  4. filtrationAfter 30 min the mixture is filtered
  5. concentrationthe filtrate is concentrated
  6. additiondiluted with Et2O
  7. customthe precipitate is collected

출처 및 근거

ORD 기록
ord-eb0c9a939d774358996ac3fe406ed8e9
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08486968B2

반응 노트

불러오는 중…