Water → HCID 76168310、化合物

HRID 639743

反応式

HRID 639743 の反応式
[C:1]([C:4]1[C:5](=[O:15])[O:6][C:7]2[CH:14]=[CH:13][CH:12]=[CH:11][C:8]=2[C:9]=1[OH:10])(=[O:3])[CH3:2].[CH3:16][O:17][CH2:18][C:19]([NH:21][C:22]1[CH:23]=[C:24]([CH:27]=[CH:28][CH:29]=1)[CH:25]=O)=[O:20].N1CCCCC1.O>C(Cl)(Cl)Cl>[OH:10][C:9]1[C:8]2[CH:11]=[CH:12][CH:13]=[CH:14][C:7]=2[O:6][C:5](=[O:15])[C:4]=1[C:1](=[O:3])[CH:2]=[CH:25][C:24]1[CH:27]=[CH:28][CH:29]=[C:22]([NH:21][C:19](=[O:20])[CH2:18][O:17][CH3:16])[CH:23]=1

参加物

6

反応物 4

HCID 962WaterHCID 8082PiperidineHCID 11615331N-(3-formylphenyl)-2-methoxyacetamideHCID 546774033-Acetyl-4-hydroxy-2H-chromen-2-one

生成物 1

HCID 76168310HCID 76168310、化合物収率 89.9%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

In 3 ml of chloroform were dissolved 0.18 g of 3-acetyl-4-hydroxy-2H-1-benzopyran-2-one, 0.17 g of 3-(methoxyacetylamino)benzaldehyde and 60 mg of piperidine, and the solution was heated under refluxing for 1 hour and 10 minutes while water was removed with a Soxhlet's extractor filled with a molecular sieve. After cooling to room temperature, the reaction solution was concentrated under reduced pressure. The residue was subjected to silica gel column chromatography, and fractions corresponding to Rf=0.3 were collected by thin layer chromatography (silica gel, chloroform (containing 2% methanol)), and concentrated to obtain 0.30 g of 4-hydroxy-3-[3-[3-(methoxyacetylamino)phenyl]-1-oxo-2-propenyl]-2H-1-benzopyran-2-one [Compound No. (21d)].

後処理

  1. temperaturethe solution was heated
  2. customwas removed with a Soxhlet's extractor
  3. additionfilled with a molecular sieve
  4. concentrationthe reaction solution was concentrated under reduced pressure
  5. customwere collected by thin layer chromatography (silica gel, chloroform (containing 2% methanol))
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-ec5447dff4b24dee9eb5599b9078be86
出典データセット
uspto-grants-2010_04
特許番号
US07691883B2

関連ノート

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