1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → HCID 10664709、化合物

HRID 984459

反応式

HRID 984459 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 10664709HCID 10664709、化合物収率 91.6%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-19fd535c4cda4ea8af4340820ac26a45
出典データセット
uspto-grants-2005_03
特許番号
US06867203B2

関連ノート

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