Dimethylformamide → HCID 765041, 화합물

HRID 1291167노트

반응식

HRID 1291167 반응식
[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]

참가 물질

4

반응물 3

HCID 6228DimethylformamideHCID 8471TriethylamineHCID 660114-Nitrobenzyl bromide

생성물 1

HCID 765041HCID 765041, 화합물

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-6f2fe62fa2a94975b3b7cdb543531a8a
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05753679

반응 노트

불러오는 중…