Dimethylformamide → Cyano-acetic acid 1-butoxycarbonyl-ethyl ester

HRID 493450

反応式

HRID 493450 の反応式
[CH2:1]([O:5][C:6](=[O:10])[CH:7]([CH3:9])[OH:8])[CH2:2][CH2:3][CH3:4].[C:11]([CH2:13][C:14](O)=[O:15])#[N:12].CN(C=O)C.C1(N=C=NC2CCCCC2)CCCCC1>CN(C)C1C=CN=CC=1.C(Cl)Cl>[CH2:1]([O:5][C:6]([CH:7]([O:8][C:14](=[O:15])[CH2:13][C:11]#[N:12])[CH3:9])=[O:10])[CH2:2][CH2:3][CH3:4]

参加物

7

反応物 4

HCID 6228DimethylformamideHCID 8738Butyl LactateHCID 9740Cyanoacetic acidHCID 10868Dicyclohexylcarbodiimide

生成物 1

HCID 23325215Cyano-acetic acid 1-butoxycarbonyl-ethyl ester

試薬・触媒・溶媒 2

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

実験手順

A mixture of 292.32 g of butyllactate, 204.14 g of cyanoacetic acid, and 14.66 g of 4-dimethylaminopyridine (DMAP) in 2000 ml of CH2Cl2 was stirred in a 3 L three-neck round bottom flask equipped with a mechanical stirrer. About 50 ml of N-N′-dimethylformide (DMF) was added to make a clear solution. The above clear solution was chilled in an ice water bath. A separately prepared dicyclohexylcarbodiimide (DCC) solution (495.19 g in 500 ml CH2Cl2) was added to the above chilled solution by using an addition funnel. White precipitate formed within five minutes after the start of the addition. The reaction mixture was left stirred overnight.

後処理

  1. customequipped with a mechanical stirrer
  2. temperatureThe above clear solution was chilled in an ice water bath
  3. customWhite precipitate formed within five minutes
  4. additionafter the start of the addition
  5. waitThe reaction mixture was left
  6. stirringstirred overnight

出典と根拠

ORDレコード
ord-67c5ae4431a242f190b4c1a3875e1265
出典データセット
uspto-grants-2009_05
特許番号
US07534907B2

関連ノート

読み込み中…