Water → 6-Allyl-piperidine-1,2-dicarboxylic acid 1-tert-butyl ester 2-methyl ester

HRID 722728노트

반응식

HRID 722728 반응식
[CH3:1][O:2][C:3]([CH:5]1[CH2:10][CH2:9][CH2:8][CH:7](OC)[N:6]1[C:13]([O:15][C:16]([CH3:19])([CH3:18])[CH3:17])=[O:14])=[O:4].[CH2:20]([Si](C)(C)C)[CH:21]=[CH2:22].B(F)(F)F.CCOCC.O>C(Cl)Cl>[CH3:1][O:2][C:3]([CH:5]1[CH2:10][CH2:9][CH2:8][CH:7]([CH2:22][CH:21]=[CH2:20])[N:6]1[C:13]([O:15][C:16]([CH3:17])([CH3:18])[CH3:19])=[O:14])=[O:4]

참가 물질

6

반응물 4

HCID 962WaterHCID 8000Boron trifluoride etherateHCID 69808AllyltrimethylsilaneHCID 670935071-Tert-butyl 2-methyl 6-methoxypiperidine-1,2-dicarboxylate

생성물 1

HCID 670930876-Allyl-piperidine-1,2-dicarboxylic acid 1-tert-butyl ester 2-methyl ester

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 6-methoxy-piperidine-1,2-dicarboxylic acid 1-tert-butyl ester 2-methyl ester, 37, (5.0 g, 18.3 mmol) and allyltrimethylsilane (5.8 mL, 36.6 mmol) in CH2Cl2 (125 mL) at −78° C. is added dropwise boron trifluoride etherate (2.5 mL, 19.7 mmol). After 1 h, the solution is poured into water and extracted with EtOAc. The extracts are washed with brine, dried (MgSO4), and concentrated in vacuo. The resulting residue is used in the next step without purification.

후처리

  1. extractionextracted with EtOAc
  2. washThe extracts are washed with brine
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated in vacuo
  5. customThe resulting residue is used in the next step without purification

출처 및 근거

ORD 기록
ord-20ebc3726ad047469049dfaf5bac238b
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07138395B2

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