Sodium Carbonate → 1-[3-(4-Tert-butylphenyl)-2-methylpropyl]piperidin-4-ol

HRID 652729

反応式

HRID 652729 の反応式
C([O-])([O-])=O.[Na+].[Na+].[C:7]([C:11]1[CH:16]=[CH:15][C:14]([CH2:17][CH:18]([CH3:21])[CH2:19]Cl)=[CH:13][CH:12]=1)([CH3:10])([CH3:9])[CH3:8].[OH:22][CH:23]1[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]1>CN(C)C=O>[C:7]([C:11]1[CH:16]=[CH:15][C:14]([CH2:17][CH:18]([CH3:21])[CH2:19][N:26]2[CH2:27][CH2:28][CH:23]([OH:22])[CH2:24][CH2:25]2)=[CH:13][CH:12]=1)([CH3:10])([CH3:9])[CH3:8]

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 79341Piperidin-4-olHCID 132518171-tert-Butyl-4-(3-chloro-2-methylpropyl)benzene

生成物 1

HCID 136076631-[3-(4-Tert-butylphenyl)-2-methylpropyl]piperidin-4-ol収率 72%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
150 °C

実験手順

106 g of Na2CO3 are added to a solution of 112 g of 3-(4-tert.-butylphenyl)-2-methyl-propyl chloride and 50 g of 4-hydroxypiperidine in 1 liter of dimethylformamide (DMF). The batch is heated at 150° C. for 15 hours and then concentrated, and the residue is taken up in CH2Cl2. The CH2CL2 phase is washed with water, dried over Na2SO4 and concentrated. Distillation of the crude product gives 103 g of N-[3-(4-tert.-butylphenyl)-2-methyl-propyl]-4-hydroxypiperidine [A] as a pale yellowish oil. Boiling point 175°-178° C./0.4 mbar.

後処理

  1. concentrationconcentrated
  2. washThe CH2CL2 phase is washed with water
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated
  5. distillationDistillation of the crude product

出典と根拠

ORDレコード
ord-ee422c24821142349a1f0d89ae2c6e72
出典データセット
uspto-grants-1987_06
特許番号
US04673683

関連ノート

読み込み中…