Water → (4-Aminomethyl-2-trifluoromethyl-phenyl)-dimethyl-amine

HRID 990876노트

반응식

HRID 990876 반응식
[CH3:1][N:2]([CH3:15])[C:3]1[CH:10]=[CH:9][C:6]([C:7]#[N:8])=[CH:5][C:4]=1[C:11]([F:14])([F:13])[F:12].[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1>[NH2:8][CH2:7][C:6]1[CH:9]=[CH:10][C:3]([N:2]([CH3:1])[CH3:15])=[C:4]([C:11]([F:12])([F:13])[F:14])[CH:5]=1

참가 물질

6

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 217328174-(Dimethylamino)-3-(trifluoromethyl)benzonitrile

생성물 1

HCID 18543285(4-Aminomethyl-2-trifluoromethyl-phenyl)-dimethyl-amine수율 46%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 4-dimethylamino-3-trifluoromethylbenzonitrile (0.35 g) in tetrahydrofuran (2 mL) is slowly added to a suspension of lithium aluminum hydride (0.1 g) in tetrahydrofuran (2 mL) at 0° C. and stirred under an atmosphere of argon for 2 hours. While at 0° C. water (0.1 mL) is slowly added followed by 5% sodium hydroxide (0.1 mL) and water (0.3 mL). The resulting gray solid is filtered and washed with tetrahydrofuran. The filtrates are collected and concentrated under reduced pressure and the resulting oil is chromatographed over silica gel (15% methanol in methylene chloride is used as the eluant) to provide the desired product as a pale orange oil (0.164 g).

후처리

  1. filtrationThe resulting gray solid is filtered
  2. washwashed with tetrahydrofuran
  3. customThe filtrates are collected
  4. concentrationconcentrated under reduced pressure
  5. customthe resulting oil is chromatographed over silica gel (15% methanol in methylene chloride

출처 및 근거

ORD 기록
ord-1d2dd6dd8d1f4d939a635f2fb6c10890
출처 데이터셋
uspto-grants-2002_10
특허 번호
US06462055B2

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