Methylamine → HCID 22139077, 화합물

HRID 18214노트

반응식

HRID 18214 반응식
Br.[NH2:2][C:3]1[C:8]([CH2:9]Br)=[CH:7][C:6]([Br:11])=[CH:5][N:4]=1.[CH3:12][NH2:13]>C1COCC1>[NH2:2][C:3]1[C:8]([CH2:9][NH:13][CH3:12])=[CH:7][C:6]([Br:11])=[CH:5][N:4]=1

참가 물질

4

반응물 2

HCID 6329MethylamineHCID 534200525-Bromo-3-(bromomethyl)pyridin-2-amine hydrobromide

생성물 1

HCID 22139077HCID 22139077, 화합물수율 80%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of the 2-amino-3-(bromomethyl)-5-bromopyridine hydrobromide salt (prepared above) in 40% aqueous methylamine (50 mL) and THF (50 mL) was stirred at RT overnight in a pressure bottle. The reaction solution was concentrated and extracted with EtOAc (2×100 mL). The combined organic phases were washed with H2O, dried over Na2SO4 and concentrated. Purification on silica gel afforded the title compound (4.25 g, 80%) as a yellow oil: MS (ES) m/e 217 (M+H)+.

후처리

  1. concentrationThe reaction solution was concentrated
  2. extractionextracted with EtOAc (2×100 mL)
  3. washThe combined organic phases were washed with H2O
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated
  6. customPurification on silica gel

출처 및 근거

ORD 기록
ord-60a395f0ce344b469af603489c0c6e46
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07741339B2

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