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

HRID 722728ノート

反応式

HRID 722728 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-20ebc3726ad047469049dfaf5bac238b
出典データセット
uspto-grants-2006_11
特許番号
US07138395B2

反応ノート

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