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Hydrazine → 2-(4-Aminomethyl-4-fluoro-piperidin-1-ylmethyl)-4,6-dichlorophenol

HRID 2112556
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HRID 2112556 반응식
NN.[Cl:3][C:4]1[C:5]([OH:31])=[C:6]([CH:27]=[C:28]([Cl:30])[CH:29]=1)[CH2:7][N:8]1[CH2:13][CH2:12][C:11]([CH2:15][N:16]2C(=O)C3C(=CC=CC=3)C2=O)([F:14])[CH2:10][CH2:9]1>C(O)C>[NH2:16][CH2:15][C:11]1([F:14])[CH2:12][CH2:13][N:8]([CH2:7][C:6]2[CH:27]=[C:28]([Cl:30])[CH:29]=[C:4]([Cl:3])[C:5]=2[OH:31])[CH2:9][CH2:10]1
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참가 물질

4

반응물 2

HCID 9321HydrazineHCID 690694182-[1-(3,5-Dichloro-2-hydroxy-benzyl)-4-fluoro-piperidin-4-ylmethyl]-isoindole-1,3-dione

생성물 1

HCID 230692642-(4-Aminomethyl-4-fluoro-piperidin-1-ylmethyl)-4,6-dichlorophenol

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Hydrazine (10 ml) was added to a solution of 2-[1-(3,5-dichloro-2-hydroxy-benzyl)-4-fluoro-piperidin-4-ylmethyl]-isoindole-1,3-dione (20.7 g) in ethanol (600 ml). The obtained solution was stirred for 5 hours while heating to reflux, and then subjected to heated filtration. The filtrate was concentrated, water was added to the residue, and then extraction with dichloromethane was followed by concentration. The obtained residue was recrystallized from isopropyl ether-pentane to obtain 2-(4-aminomethyl-4-fluoro-piperidin-1-ylmethyl)-4,6-dichlorophenol.

후처리

  1. temperaturewhile heating
  2. temperatureto reflux
  3. temperatureto heated
  4. filtrationfiltration
  5. concentrationThe filtrate was concentrated
  6. additionwater was added to the residue
  7. extractionextraction with dichloromethane
  8. concentrationwas followed by concentration
  9. customThe obtained residue was recrystallized from isopropyl ether-pentane

출처 및 근거

ORD 기록
ord-a60542660a33494fba249a1c7dac629b
출처 데이터셋
uspto-grants-2009_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07524841B2

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