Dimethylformamide → HCID 765041、化合物

HRID 1291167ノート

反応式

HRID 1291167 の反応式
[N+:1]([C:4]1[CH:11]=[CH:10][C:7]([CH2:8]Br)=[CH:6][CH:5]=1)([O-:3])=[O:2].C([N:14]([CH2:17][CH3:18])[CH2:15][CH3:16])C.CN(C)[CH:21]=[O:22]>>[N+:1]([C:4]1[CH:11]=[CH:10][C:7]([CH2:8][N:14]2[CH2:15][CH2:16][CH:21]([OH:22])[CH2:18][CH2:17]2)=[CH:6][CH:5]=1)([O-:3])=[O:2]

参加物

4

反応物 3

HCID 6228DimethylformamideHCID 8471TriethylamineHCID 660114-Nitrobenzyl bromide

生成物 1

HCID 765041HCID 765041、化合物

実験手順

1.0 g (0.00989 mol) of 4-hydroxypiperidi,ne was dissolved in 50 ml of dimethylformamide and cooled to 0°. 2.56g (0.001186 mol) of 4-nitro-benzyl bromide and 2.78 ml (0.0198 mol) of triethylamine were added and the mixture was left to come to room temperature. It was stirred for 16 hrs., the solvent was distilled off and the residue was taken up in dichloromethane. The organic phase was washed with water and saturated sodium chloride solution, dried over magnesium sulfate and concentrated and the residue was chromatographed on silica gel with dichloromethane/methanol (9:1) as the eluent. 0.836 g (36%) of 1-(4-nitro-benzyl-piperidin-4-ol was obtained as beige crystals; m.p. 114°-115°.

後処理

  1. temperaturecooled to 0°
  2. waitthe mixture was left
  3. customto come to room temperature
  4. distillation, the solvent was distilled off
  5. washThe organic phase was washed with water and saturated sodium chloride solution
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated
  8. customthe residue was chromatographed on silica gel with dichloromethane/methanol (9:1) as the eluent

出典と根拠

ORDレコード
ord-6f2fe62fa2a94975b3b7cdb543531a8a
出典データセット
uspto-grants-1998_05
特許番号
US05753679

反応ノート

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