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

HRID 57641ノート

反応式

HRID 57641 の反応式
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

参加物

6

反応物 4

HCID 260Hydrogen Bromide2 回HCID 14798Sodium HydroxideHCID 167921071-(4-Aminophenyl)piperidin-4-olHCID 23668193Sodium Nitrite

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ecdf40fd281e46aeb409fcdd9637bab6
出典データセット
uspto-grants-2016_09
特許番号
US09434726B2

反応ノート

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