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Ethanol → HCID 14551199、化合物

HRID 1165898
ノート
印刷プレビュー

反応式

HRID 1165898 の反応式
C(=O)[CH2:2][CH:3]([CH3:5])[CH3:4].N1CCOCC1.C(O)C.[CH3:16][O:17][C:18]([C:20]1[C:24](=O)O[C:22]2=[CH:26][CH:27]=[C:28]([CH:31]([CH3:33])[CH3:32])[CH:29]=[CH:30][C:21]=12)=[O:19]>C1(C)C=CC=CC=1>[CH3:16][O:17][C:18]([C:20]1[C:21]2[C:22]([CH:26]=[CH:27][C:28]([CH:31]([CH3:33])[CH3:32])=[CH:29][CH:30]=2)=[C:2]([CH:3]([CH3:5])[CH3:4])[CH:24]=1)=[O:19]
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 702EthanolHCID 8083MorpholineHCID 115523-MethylbutanalHCID 14515736HCID 14515736、化合物

生成物 1

HCID 14551199HCID 14551199、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

Isovaleraldehyde (5.16 g) and morpholine (4.36 g) are added to ethanol (14 ml) and then 3-methoxycarbonyl-6-isopropyl-2H-cyclohepta[b]furan-2-one (5) (2.46 g) is added thereto. The obtained mixture is heated under reflux for 16 hours, and then the solvent is distilled off under reduced pressure to give an oily material. The obtained oily material is dissolved in toluene (20 ml), washed twice with water (20 ml) and 4 times with 1N HCl (20 ml), and further, twice with water (40 ml). The obtained toluene layer is passed through silica gel column (1.05 kg), the column is eluted with toluene. From the eluted parts including the product (24), the solvent is distilled off under reduced pressure to give the compound (24) as a purple oily material in a yield of 2.08 g, 76.%.

後処理

  1. temperatureThe obtained mixture is heated
  2. temperatureunder reflux for 16 hours
  3. distillationthe solvent is distilled off under reduced pressure
  4. customto give an oily material
  5. washwashed twice with water (20 ml) and 4 times with 1N HCl (20 ml)
  6. washthe column is eluted with toluene
  7. distillationthe solvent is distilled off under reduced pressure

出典と根拠

ORDレコード
ord-82945cad1443406f8f5976df7afb2267
出典データセット
uspto-grants-1990_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04912134

反応ノート

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