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HCID 19861151, 화합물 → HCID 12877973, 화합물

HRID 2291121
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HRID 2291121 반응식
[N:1]1([CH:6]([CH2:16][CH2:17][CH2:18][CH3:19])[C:7]([C:9]2[CH:14]=[CH:13][C:12]([Cl:15])=[CH:11][CH:10]=2)=[O:8])[CH:5]=[N:4][CH:3]=[N:2]1.[H-].[Al+3].[Li+].[H-].[H-].[H-]>C(OCC)C>[N:1]1([CH:6]([CH2:16][CH2:17][CH2:18][CH3:19])[CH:7]([C:9]2[CH:14]=[CH:13][C:12]([Cl:15])=[CH:11][CH:10]=2)[OH:8])[CH:5]=[N:4][CH:3]=[N:2]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 19861151HCID 19861151, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 12877973HCID 12877973, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

The product (0.01 mol) of Stage 2 was added portionwise to a suspension of lithium aluminium hydride (0.005 mol) in diethyl ether (10 ml; dried over sodium) to maintain refluxing. The ethereal solution was refluxed for a further four hours; the excess lithium aluminium hydride was quenched with water (20.0 ml) and the mixture acidified with concentrated sulphuric acid. The ethereal layer was washed with water (4×25 ml) and dried over anhydrous sodium sulphate. Removal of the ether gave an oil which solidified on standing. Recrystallisation from methylene chloride/petroleum ether gave the title compound as a white solid, m.p. 93°-94°.

후처리

  1. temperatureto maintain
  2. temperaturerefluxing
  3. temperatureThe ethereal solution was refluxed for a further four hours
  4. customthe excess lithium aluminium hydride was quenched with water (20.0 ml)
  5. washThe ethereal layer was washed with water (4×25 ml)
  6. dry with materialdried over anhydrous sodium sulphate
  7. customRemoval of the ether
  8. customgave an oil which
  9. customRecrystallisation from methylene chloride/petroleum ether

출처 및 근거

ORD 기록
ord-0b0deadf62f343bc9e13f7cfb1f0e943
출처 데이터셋
uspto-grants-1986_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04620011

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