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

HRID 652729노트

반응식

HRID 652729 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
150 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-ee422c24821142349a1f0d89ae2c6e72
출처 데이터셋
uspto-grants-1987_06
특허 번호
US04673683

반응 노트

불러오는 중…