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Ethyl chloroacetate → ethyl [4-[(Z)-2-cyano-2-(3,4-dimethoxy-phenyl)-vinyl]-phenoxy]-acetate

HRID 2222356
ノート
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反応式

HRID 2222356 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5](/[C:11](=[CH:14]/[C:15]2[CH:20]=[CH:19][C:18]([OH:21])=[CH:17][CH:16]=2)/[C:12]#[N:13])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].Cl[CH2:23][C:24]([O:26][CH2:27][CH3:28])=[O:25].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[C:12](/[C:11](/[C:5]1[CH:6]=[CH:7][C:8]([O:9][CH3:10])=[C:3]([O:2][CH3:1])[CH:4]=1)=[CH:14]\[C:15]1[CH:16]=[CH:17][C:18]([O:21][CH2:23][C:24]([O:26][CH2:27][CH3:28])=[O:25])=[CH:19][CH:20]=1)#[N:13]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 7751Ethyl chloroacetateHCID 11430Potassium CarbonateHCID 10446442(Z)-2-(3,4-dimethoxyphenyl)-3-(4-hydroxyphenyl)acrylonitrile

生成物 1

HCID 10384323ethyl [4-[(Z)-2-cyano-2-(3,4-dimethoxy-phenyl)-vinyl]-phenoxy]-acetate収率 34%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

Compound 1 (281 mg) and ethyl chloroacetate (245 mg) were dissolved in acetone, and potassium carbonate was added to the resultant solution, followed by reflux for three hours. The resultant mixture was subjected to filtration, and insoluble matter was removed from the mixture. The resultant filtrate was concentrated to dryness under reduced pressure, followed by recrystallization, to thereby produce the target product (124 mg, yield: 34%).

後処理

  1. temperatureby reflux for three hours
  2. filtrationThe resultant mixture was subjected to filtration, and insoluble matter
  3. customwas removed from the mixture
  4. concentrationThe resultant filtrate was concentrated to dryness under reduced pressure
  5. customfollowed by recrystallization

出典と根拠

ORDレコード
ord-2102ffc89b3b428fb6e9eec6dc6fcac6
出典データセット
uspto-grants-2008_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07371773B2

反応ノート

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