Iodoethane → Tert-butyl 3-ethoxy-4,4-dimethoxypiperidine-1-carboxylate

HRID 1425123노트

반응식

HRID 1425123 반응식
[OH:1][CH:2]1[C:7]([O:10][CH3:11])([O:8][CH3:9])[CH2:6][CH2:5][N:4]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH2:3]1.[H-].[Na+].I[CH2:22][CH3:23]>CN(C=O)C>[CH2:22]([O:1][CH:2]1[C:7]([O:8][CH3:9])([O:10][CH3:11])[CH2:6][CH2:5][N:4]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH2:3]1)[CH3:23]

참가 물질

5

반응물 3

HCID 6340IodoethaneHCID 24758Sodium hydrideHCID 11425480Tert-butyl 3-hydroxy-4,4-dimethoxypiperidine-1-carboxylate

생성물 1

HCID 68406637Tert-butyl 3-ethoxy-4,4-dimethoxypiperidine-1-carboxylate수율 84.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

The same operation as in Example (90a) was performed using tert-butyl 3-hydroxy-4,4-dimethoxypiperidine-1-carboxylate (5.2 g, 20 mmol), sodium hydride (55% content, 1.31 g, 30 mmol), 1-iodoethane (6.24 g, 40 mmol) and DMF (50 mL). The residue was purified by silica gel column chromatography (elution solvent: hexane/ethyl acetate=10/1, 4/1, 2/1) to obtain 4.90 g of the title compound as a colorless oily substance (85%).

후처리

  1. customThe residue was purified by silica gel column chromatography (elution solvent: hexane/ethyl acetate=10/1, 4/1, 2/1)

출처 및 근거

ORD 기록
ord-1a7aab3c735142d48fb1a14ab914dbfa
출처 데이터셋
uspto-grants-2015_01
특허 번호
US08927588B2

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