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

HRID 493450

반응식

HRID 493450 반응식
[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]

참가 물질

7

반응물 4

HCID 6228DimethylformamideHCID 8738Butyl LactateHCID 9740Cyanoacetic acidHCID 10868Dicyclohexylcarbodiimide

생성물 1

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

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-67c5ae4431a242f190b4c1a3875e1265
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07534907B2

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