1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → HCID 10664709, 화합물

HRID 984459

반응식

HRID 984459 반응식
[Cl:1][C:2]1[CH:12]=[CH:11][C:5](/[CH:6]=[CH:7]/[C:8]([OH:10])=O)=[CH:4][C:3]=1[N+:13]([O-:15])=[O:14].[C:16]([N:19]1[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1)(=[O:18])[CH3:17].CCN=C=NCCCN(C)C>CN(C=O)C>[Cl:1][C:2]1[CH:12]=[CH:11][C:5](/[CH:6]=[CH:7]/[C:8]([N:22]2[CH2:23][CH2:24][N:19]([C:16](=[O:18])[CH3:17])[CH2:20][CH2:21]2)=[O:10])=[CH:4][C:3]=1[N+:13]([O-:15])=[O:14]

참가 물질

5

반응물 3

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 837951-AcetylpiperazineHCID 6881084-Chloro-3-nitrocinnamic Acid

생성물 1

HCID 10664709HCID 10664709, 화합물수율 91.6%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a stirred solution of trans-4-chloro-3-nitrocinnamic acid (1.50 g, 6.59 mmol) and 1-acetylpiperazine (0.89 g, 6.94 mmol) in 20 mL of DMF at room temperature was added EDAC (1.4 g, 7.30 mmol). The mixture was then stirred at room temperature for 2 hours. TLC indicated the complete consumption of the acid. Water was then added to quench the reaction and to precipitate out the product. Cinnamide was then collected through filtration and washed with cold water. The light yellow product was dried in vacuum oven overnight at 40° C. to give 2.04 g (6.03 mmol, 91.6%) of the title compound.

후처리

  1. customthe complete consumption of the acid
  2. additionWater was then added
  3. customto quench
  4. customthe reaction
  5. customto precipitate out the product
  6. filtrationCinnamide was then collected through filtration
  7. washwashed with cold water
  8. customThe light yellow product was dried in vacuum oven overnight at 40° C.

출처 및 근거

ORD 기록
ord-19fd535c4cda4ea8af4340820ac26a45
출처 데이터셋
uspto-grants-2005_03
특허 번호
US06867203B2

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