Water → 3,3-Dimethylbutyl 3-piperidinopropyl ether

HRID 1376164ノート

反応式

HRID 1376164 の反応式
[N:1]1([CH2:7][CH2:8][CH2:9][O-:10])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[Na+].[CH3:12][C:13]([CH3:18])([CH3:17])[CH2:14][CH2:15]Cl.C1OCCOCCOCCOCCOC1.O>[I-].C([N+](CCCC)(CCCC)CCCC)CCC.CS(C)=O>[N:1]1([CH2:7][CH2:8][CH2:9][O:10][CH2:15][CH2:14][C:13]([CH3:18])([CH3:17])[CH3:12])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

参加物

7

反応物 4

HCID 962WaterHCID 3633615-Crown-5HCID 761111-Chloro-3,3-dimethylbutaneHCID 23694275HCID 23694275、化合物

生成物 1

HCID 97945573,3-Dimethylbutyl 3-piperidinopropyl ether

試薬・触媒・溶媒 2

HCID 67553Tetrabutylammonium Iodide触媒HCID 679Dimethyl Sulfoxide溶媒

実験手順

Sodium 3-piperidinopropanolate (5 mmol), 5 mmol of 3,3-dimethylbutyl chloride, a catalytic amount of tetrabutylammonium iodide, and 0.5 mmol of 15-crown-5 in 10 ml of dry dimethyl sulfoxide were refluxed for 12 hours. Water was added, and it was extracted with diethyl ether. The organic layer was purified by column chromatography on silica gel (eluent: methylene chloride/methanol (90/10), ammonia atmosphere). The solvent was removed under reduced pressure and the residue crystallized with oxalic acid from diethyl ether/ethanol.

後処理

  1. extractionit was extracted with diethyl ether
  2. customThe organic layer was purified by column chromatography on silica gel (eluent: methylene chloride/methanol (90/10), ammonia atmosphere)
  3. customThe solvent was removed under reduced pressure
  4. customthe residue crystallized with oxalic acid from diethyl ether/ethanol

出典と根拠

ORDレコード
ord-8d5875571de64e99b721756f1b8bfbe6
出典データセット
uspto-grants-2007_01
特許番号
US07169928B2

反応ノート

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