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Ethanol → HCID 14551199, 화합물

HRID 1165898
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HRID 1165898 반응식
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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 702EthanolHCID 8083MorpholineHCID 115523-MethylbutanalHCID 14515736HCID 14515736, 화합물

생성물 1

HCID 14551199HCID 14551199, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.%.

후처리

  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

출처 및 근거

ORD 기록
ord-82945cad1443406f8f5976df7afb2267
출처 데이터셋
uspto-grants-1990_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04912134

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