tert-Butanol → HCID 21287969、化合物

HRID 868352ノート

反応式

HRID 868352 の反応式
[CH3:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][N:3]=1.[C:11](O)([CH3:14])([CH3:13])[CH3:12].Cl.C(N=C=NCCCN(C)C)C>CN(C)C1C=CN=CC=1.ClCCl>[CH3:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([O:8][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:7])=[CH:4][N:3]=1

参加物

6

反応物 3

HCID 6386tert-ButanolHCID 1378606-Methylnicotinic acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride

生成物 1

HCID 21287969HCID 21287969、化合物収率 44.6%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒

実験手順

A mixture of 11.3 g of 6-methylnicotinic acid, 5.0 g of 4-dimethylaminopyridine, 18.3 g of t-butyl alcohol, 22.4 g of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride, and 280 ml of dichloromethane is stirred at room temperature for 2 days. The reaction mixture is washed with water, dried over magnesium sulfate, and concentrated. The residue is chromatographed on silica gel with chloroform to give 7.1 g of t-butyl 6-methylnicotinate as an oil.

後処理

  1. washThe reaction mixture is washed with water
  2. dry with materialdried over magnesium sulfate
  3. concentrationconcentrated
  4. customThe residue is chromatographed on silica gel with chloroform

出典と根拠

ORDレコード
ord-c808eedd4345449aa05091cffa6f4ee4
出典データセット
uspto-grants-1988_10
特許番号
US04778796

反応ノート

読み込み中…