(6-Bromo-5-fluoropyridin-2-yl)-tert-butylamine → 6-Bromo-5-fluoropyridin-2-amine

HRID 1945595

반응식

HRID 1945595 반응식
[Br:1][C:2]1[N:7]=[C:6]([NH:8]C(C)(C)C)[CH:5]=[CH:4][C:3]=1[F:13]>ClCCCl.C(O)(C(F)(F)F)=O>[Br:1][C:2]1[N:7]=[C:6]([NH2:8])[CH:5]=[CH:4][C:3]=1[F:13]

참가 물질

4

반응물 1

HCID 59605446(6-Bromo-5-fluoropyridin-2-yl)-tert-butylamine

생성물 1

HCID 596058336-Bromo-5-fluoropyridin-2-amine수율 71%

시약·촉매·용매 2

HCID 111,2-Dichloroethane용매HCID 6422Trifluoroacetic acid용매

실험 절차

A solution of (6-bromo-5-fluoropyridin-2-yl)-tert-butylamine (46 mg, 0.19 mmol) in DCE (2 mL) and TFA (2 mL) was heated at 120° C. for 10 min in a microwave reactor, and then concentrated under reduced pressure. The residue was taken up in MeOH and loaded onto an Isolute® SCX-2 cartridge (5 g). The cartridge was washed with MeOH then the desired product eluted with 2 M NH3 in MeOH to give 6-Bromo-5-fluoropyridin-2-ylamine as an off-white solid (25 mg, 71%). 1H NMR (400 MHz, CHCl3-d): δ 7.21 (dd, J=8.7, 7.2 Hz, 1 H); 6.39 (dd, J=8.7, 2.7 Hz, 1 H); 4.89-3.75 (s, 2 H).

후처리

  1. concentrationconcentrated under reduced pressure
  2. washThe cartridge was washed with MeOH
  3. washthe desired product eluted with 2 M NH3 in MeOH

출처 및 근거

ORD 기록
ord-6ff17c1b88be409991979326ec296f80
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08394796B2

연결된 노트

불러오는 중…