1-Methylpiperazine → [2-(4-Methylpiperazino)-5-nitrophenyl]methanol

HRID 1190863노트

반응식

HRID 1190863 반응식
F[C:2]1[CH:9]=[CH:8][C:7]([N+:10]([O-:12])=[O:11])=[CH:6][C:3]=1[CH2:4][OH:5].[CH3:13][N:14]1[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]1>C1COCC1>[CH3:13][N:14]1[CH2:19][CH2:18][N:17]([C:2]2[CH:9]=[CH:8][C:7]([N+:10]([O-:12])=[O:11])=[CH:6][C:3]=2[CH2:4][OH:5])[CH2:16][CH2:15]1

참가 물질

4

반응물 2

HCID 531671-MethylpiperazineHCID 4437169(2-Fluoro-5-nitrophenyl)methanol

생성물 1

HCID 25918812[2-(4-Methylpiperazino)-5-nitrophenyl]methanol수율 94%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

2-Fluoro-5-nitrobenzyl alcohol (1 g, 5.84 mmol) and N-methylpiperazine (1.29 mL, 2 eq) were heated at 130° C. for 1 h. The reaction mixture was then diluted with 25 mL of THF and washed with a saturated aqueous solution of Na2CO3 and then with brine. The organic layer was dried over Na2SO4, filtered and evaporated. The residue was thoroughly washed with pentane and filtered off to yield expected compound as an orange powder (1.38 g, 94% yield). m/z (ESI) 252.1 [M+H]+.

후처리

  1. washwashed with a saturated aqueous solution of Na2CO3
  2. dry with materialThe organic layer was dried over Na2SO4
  3. filtrationfiltered
  4. customevaporated
  5. washThe residue was thoroughly washed with pentane
  6. filtrationfiltered off

출처 및 근거

ORD 기록
ord-a7a4d715d5a94319bcd29bd81c8f21d4
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08680095B2

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