Cyclobutylamine → 5-bromo-N-cyclobutylpyridin-3-amine

HRID 445728

반응식

HRID 445728 반응식
[Br:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6](F)[CH:7]=1.[CH:9]1([NH2:13])[CH2:12][CH2:11][CH2:10]1>CN1C(=O)CCC1.CCOC(C)=O>[Br:1][C:2]1[CH:7]=[C:6]([NH:13][CH:9]2[CH2:12][CH2:11][CH2:10]2)[CH:5]=[N:4][CH:3]=1

참가 물질

5

반응물 2

HCID 75645CyclobutylamineHCID 8202063-Bromo-5-fluoropyridine

생성물 1

HCID 596199875-bromo-N-cyclobutylpyridin-3-amine

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 13387N-methyl-2-pyrrolidone용매

반응 조건

온도
200 °C

실험 절차

A mixture of 3-bromo-5-fluoropyridine (Frontier Scientific, Logan, USA, 5.63 mmol) and cyclobutylamine (Fluka, Buchs, Switzerland, 12.38 mmol) in NMP (8 ml) was heated under microwave irradiation for 1 h at 190° C. and for 5.5 h at 200° C. The reaction mixture was diluted with EtOAc and washed with saturated aqueous NaHCO3, with brine (3×), dried over Na2SO4, filtered, evaporated and dried under vacuum to give the title compound as an off-white solid. (HPLC: tR 2.31 min (Method A); M+H=227, 229 MS-ES)

후처리

  1. washwashed with saturated aqueous NaHCO3, with brine (3×)
  2. dry with materialdried over Na2SO4
  3. filtrationfiltered
  4. customevaporated
  5. customdried under vacuum

출처 및 근거

ORD 기록
ord-1c537545f2964122a62d2fd303c60f36
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08476294B2

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