Water → 1-(Naphthalen-2-yl)ethan-1-amine

HRID 559125

반응식

HRID 559125 반응식
[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[C@H:11]([NH2:13])[CH3:12].C(=O)([O-])[O-].[Cs+].[Cs+].O>O1CCOCC1.C(Cl)Cl>[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[CH:11]([NH2:13])[CH3:12]

참가 물질

6

반응물 3

HCID 962WaterHCID 10796Cesium carbonateHCID 1798835(1R)-1-(naphthalen-2-yl)ethan-1-amine

생성물 1

HCID 38571451-(Naphthalen-2-yl)ethan-1-amine

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 312751,4-Dioxane용매

반응 조건

온도
80 °C

실험 절차

A mixture of (R)-(+)-1-(2-napthyl)ethylamine (102.6 mg, 0.599 mmol), 2,4-dichloro-5-fluororo pyrimidine (100 mg, 0.599 mmol) and cesium carbonate (390 mg, 1.2 mmol) was dissolved in 1,4-dioxane (3 ml) and H2O (3 ml) in a 10 ml microwave vial. The mixture was stirred in the microwave reactor at 80° C. for 10 minutes. The residue was dissolved in CH2Cl2 (50 ml), washed with water (20 ml), brine (20 ml) dried (Na2SO4) and concentrated to get the crude intermediate 2-chloro-5-fluoro-pyrimidin-4-yl)-(1-naphthalen-2-yl-ethyl)-amine.

후처리

  1. washwashed with water (20 ml), brine (20 ml)
  2. dry with materialdried (Na2SO4)
  3. concentrationconcentrated

출처 및 근거

ORD 기록
ord-8ca4602e8a334118a865928edefdc391
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08063057B2

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