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

HRID 1190863ノート

反応式

HRID 1190863 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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]+.

後処理

  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

出典と根拠

ORDレコード
ord-a7a4d715d5a94319bcd29bd81c8f21d4
出典データセット
uspto-grants-2014_03
特許番号
US08680095B2

反応ノート

読み込み中…