Hydrogen Bromide → 1-(4-Bromophenyl)piperidin-4-ol

HRID 57641노트

반응식

HRID 57641 반응식
N[C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:13][CH2:12][CH:11]([OH:14])[CH2:10][CH2:9]2)=[CH:4][CH:3]=1.N([O-])=O.[Na+].[OH-].[Na+].[BrH:21]>O>[Br:21][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:13][CH2:12][CH:11]([OH:14])[CH2:10][CH2:9]2)=[CH:4][CH:3]=1

참가 물질

6

반응물 4

HCID 260Hydrogen Bromide2회HCID 14798Sodium HydroxideHCID 167921071-(4-Aminophenyl)piperidin-4-olHCID 23668193Sodium Nitrite

생성물 1

HCID 235052161-(4-Bromophenyl)piperidin-4-ol

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
0 °C

실험 절차

1-(4-aminophenyl)piperidin-4-ol (600 mg, 3.12 mmol), HBr (14 mL, 48%), was mixed and cooled to 0° C., the solution of NaNO2 (215 mg, 3.12 mmol) in 2.3 mL water was added in. the mixture was stirred for 15 minutes, the solution of CuBr (246 mg, 1.72 mmol) in HBr (4.4 mL 4.8%) was added and reacted at 100° C. for 3 hours. 2M NaOH solution was added, extracted by EA, washed by 2M NaOH, dried over Na2SO4, concentrated and purified by flash chromatography. (PE:EA=3:1) to give 520 mg pale brown solid.

후처리

  1. customreacted at 100° C. for 3 hours
  2. extractionextracted by EA
  3. washwashed by 2M NaOH
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated
  6. custompurified by flash chromatography

출처 및 근거

ORD 기록
ord-ecdf40fd281e46aeb409fcdd9637bab6
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09434726B2

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