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Ethanolamine → 2-((6-Chloropyrazin-2-yl)amino)ethanol

HRID 1774750
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HRID 1774750 반응식
Cl[C:2]1[CH:7]=[N:6][CH:5]=[C:4]([Cl:8])[N:3]=1.[NH2:9][CH2:10][CH2:11][OH:12].CCN(C(C)C)C(C)C>C(O)CCC>[Cl:8][C:4]1[N:3]=[C:2]([NH:9][CH2:10][CH2:11][OH:12])[CH:7]=[N:6][CH:5]=1
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참가 물질

5

반응물 3

HCID 700EthanolamineHCID 785042,6-DichloropyrazineHCID 81531Diisopropylethylamine

생성물 1

HCID 534088382-((6-Chloropyrazin-2-yl)amino)ethanol수율 50%

시약·촉매·용매 1

HCID 2631-Butanol용매

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온도
80 °C

실험 절차

In a sealed tube, 2,6-dichloropyrazine (1 g, 6.71 mmol) was mixed with 2-aminoethanol (0.492 g, 8.05 mmol), Hunig's base (1.13 g, 8.73 mmol) in BuOH (7 mL) and the reaction mixture was heated to 80° C. over night. The mixture was concentrated in vacuo and the residue partitioned between NaHCO3 (20 mL) and EtOAc (100 mL). The organic phase was separated, washed with brine, dried over Na2SO4, filtered and evaporated to dryness to give the title compound (0.583 g, 50%) as a light yellow foam. MS: 174.1 (M+H+).

후처리

  1. concentrationThe mixture was concentrated in vacuo
  2. customthe residue partitioned between NaHCO3 (20 mL) and EtOAc (100 mL)
  3. customThe organic phase was separated
  4. washwashed with brine
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. customevaporated to dryness

출처 및 근거

ORD 기록
ord-0651662b5f2445acb5803f7bbfa2290b
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09260408B2

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