Pyridine → (3-Ethyloxetan-3-yl)methyl 3-pyridinecarboxylate

HRID 345288

反応式

HRID 345288 の反応式
Cl.[CH2:2](Cl)[C:3]1[CH:8]=[CH:7][CH:6]=[N:5][CH:4]=1.[CH2:10]([C:12]1([CH2:16][OH:17])[CH2:15][O:14][CH2:13]1)[CH3:11].N1C=CC=CC=1.C(=O)([O-])[O-:25].[Na+].[Na+]>ClCCl>[N:5]1[CH:6]=[CH:7][CH:8]=[C:3]([C:2]([O:17][CH2:16][C:12]2([CH2:10][CH3:11])[CH2:15][O:14][CH2:13]2)=[O:25])[CH:4]=1

参加物

6

反応物 4

HCID 1049PyridineHCID 10340Sodium CarbonateHCID 233943-(Chloromethyl)pyridine hydrochlorideHCID 76444Oxt-101

生成物 1

HCID 19992002(3-Ethyloxetan-3-yl)methyl 3-pyridinecarboxylate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Nicotinyl chloride hydrochloride (8.9 gm.) was added to a stirred solution of 3-ethyl-3-hydroxymethyloxetane (5.8 gm.) and dry pyridine (20 ml.) in dry dichloromethane (150 ml.) at 0°. The mixture was stirred at room temperature for 4 days and poured into aqueous sodium carbonate solution. The aqueous mixture was extracted with dichloromethane. The extracts were washed with water and dried over anhydrous magnesium sulphate. The solvent was removed in vacuo. The residue was purified by chromatography on silica eluting with 5% triethylamine in dichloromethane. (3-Ethyloxetan-3-yl)methyl 3-pyridinecarboxylate was obtained as a pale yellow oil (7.0 gm.).

後処理

  1. extractionThe aqueous mixture was extracted with dichloromethane
  2. washThe extracts were washed with water
  3. dry with materialdried over anhydrous magnesium sulphate
  4. customThe solvent was removed in vacuo
  5. customThe residue was purified by chromatography on silica eluting with 5% triethylamine in dichloromethane

出典と根拠

ORDレコード
ord-e348c7bc47ba44ad998de5232bb87078
出典データセット
uspto-grants-1991_10
特許番号
US05057504

関連ノート

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