Ethyl 2-amino-2-(5-bromo-3-chloropyridin-2-yl)acetate → (5-Bromo-3-chloropyridin-2-yl)methanamine hydrochloride

HRID 1502722노트

반응식

HRID 1502722 반응식
[NH2:1][CH:2]([C:8]1[C:13]([Cl:14])=[CH:12][C:11]([Br:15])=[CH:10][N:9]=1)C(OCC)=O>Cl>[ClH:14].[Br:15][C:11]1[CH:12]=[C:13]([Cl:14])[C:8]([CH2:2][NH2:1])=[N:9][CH:10]=1

참가 물질

3

반응물 1

HCID 71138503Ethyl 2-amino-2-(5-bromo-3-chloropyridin-2-yl)acetate

생성물 1

HCID 71138342(5-Bromo-3-chloropyridin-2-yl)methanamine hydrochloride수율 182.4%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

A stirred solution of ethyl 2-amino-2-(5-bromo-3-chloropyridin-2-yl)acetate (0.5 g, 1.7 mmol) in 3 N HCl (25 mL) was heated at reflux for 4 h. The reaction mixture was washed with diethyl ether and H2O. The combined ether layer was concentrated under reduced pressure to afford the title compound as an off-white solid (400 mg, 65%): 1H NMR (400 MHz, CDCl3) δ 8.78 (s, 1H), 8.70 (br s, 2H), 8.45 (s, 1H), 4.56 (m, 2H); ESIMS m/z 221.15 ([M+H]+).

후처리

  1. temperatureat reflux for 4 h
  2. washThe reaction mixture was washed with diethyl ether and H2O
  3. concentrationThe combined ether layer was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-979e05748d3c4e4ea9b7decb1fc887fd
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09210927B2

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