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Water → HCID 45117061、化合物

HRID 2111003
ノート
印刷プレビュー

反応式

HRID 2111003 の反応式
[CH:1]1[C:6]([CH2:7][Cl:8])=[CH:5][CH:4]=[C:3](/[C:9](/Cl)=[N:10]\[OH:11])[CH:2]=1.CO[CH:15]=[CH:16][C:17]([O:19][CH3:20])=[O:18].C(N(CC)CC)C.O>ClCCl>[Cl:8][CH2:7][C:6]1[CH:5]=[CH:4][C:3]([C:9]2[C:16]([C:17]([O:19][CH3:20])=[O:18])=[CH:15][O:11][N:10]=2)=[CH:2][CH:1]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 2724617Methyl 3-methoxyprop-2-enoateHCID 91622765HCID 91622765、化合物

生成物 1

HCID 45117061HCID 45117061、化合物収率 51.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

N-Hydroxy-4-chloromethylbenzenecarboxyimidoyl chloride (15.27 g, 74.82 mmol) was dissolved in dichloromethane (300 ml), methyl 3-methoxyacrylate (10.43 g, 89.82 mmol) was added, and triethylamine (21 ml, 151 mmol) was slowly added dropwise. The mixture was stirred overnight at room temperature. Water was added, and the mixture was extracted with dichloromethane. The extract was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the obtained crude product was purified by silica gel chromatography (hexane:ethyl acetate=5:1) to give the title compound (9.67 g, 51%).

後処理

  1. extractionthe mixture was extracted with dichloromethane
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customthe obtained crude product
  6. customwas purified by silica gel chromatography (hexane:ethyl acetate=5:1)

出典と根拠

ORDレコード
ord-a3a1861b58df4dc7b771d683206694cb
出典データセット
uspto-grants-2009_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07517996B2

反応ノート

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