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Water → HCID 18689383, 화합물

HRID 1871839
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HRID 1871839 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][O:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[O:16][C:17]3[CH:25]=[CH:24][CH:23]=[CH:22][C:18]=3[C:19](=O)[N:20]=2)=[CH:11][CH:10]=1.[CH:26]12[CH2:35][CH:30]3[CH2:31][CH:32]([CH2:34][CH:28]([CH2:29]3)[C:27]1=O)[CH2:33]2.O>C1COCC1.[Cl-].[Ti+4].[Cl-].[Cl-].[Cl-].C(OCC)(=O)C>[CH:26]12[CH2:35][CH:30]3[CH2:31][CH:32]([CH2:34][CH:28]([CH2:29]3)[C:27]1=[C:19]1[C:18]3[CH:22]=[CH:23][CH:24]=[CH:25][C:17]=3[O:16][C:15]([C:12]3[CH:13]=[CH:14][C:9]([O:8][CH3:7])=[CH:10][CH:11]=3)=[N:20]1)[CH2:33]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 962WaterHCID 64151AdamantanoneHCID 776579HCID 776579, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 18689383HCID 18689383, 화합물

시약·촉매·용매 3

HCID 160960Diamminetetrachlorotitanate(IV)촉매
HCID 8028
Tetrahydrofuran
용매
HCID 8857Ethyl Acetate용매

실험 절차

21 mmol lithium aluminium hydride is carefully added to a suspension of 40 mmol titanium chloride in 100 ml absolute THF while stirring vigorously. After stirring for 1 hour at room temperature, a mixture of 15 mmol 2-(4'-methoxyphenyl)-4H-1,3-benzoxazine-4-one and 11 mmol adamantanone is added while cooling on ice. It is heated to boiling for 60 min under reflux. After cooling to room temperature it is poured onto 200 ml water. The mixture is shaken out twice with 200 ml ethyl acetate each time. The combined organic phases are washed once with water and separated. After drying over sodium sulfate it is filtered and the solvent is removed by distillation. The oily residue is separated by column chromatography (silica gel: ethyl acetate/petroleum ether 1:9).

후처리

  1. stirringAfter stirring for 1 hour at room temperature
  2. additionis added
  3. temperaturewhile cooling on ice
  4. temperatureIt is heated
  5. temperatureunder reflux
  6. washThe combined organic phases are washed once with water
  7. customseparated
  8. dry with materialAfter drying over sodium sulfate it
  9. filtrationis filtered
  10. customthe solvent is removed by distillation
  11. customThe oily residue is separated by column chromatography (silica gel: ethyl acetate/petroleum ether 1:9)

출처 및 근거

ORD 기록
ord-ff6363ccc5b945cfac88be3fee219ef2
출처 데이터셋
uspto-grants-2000_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06107036

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