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HCID 19861151、化合物 → HCID 12877973、化合物

HRID 2308701
ノート
印刷プレビュー

反応式

HRID 2308701 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 19861151HCID 19861151、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 12877973HCID 12877973、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-72ec75b9fd12409e84f0ac8ae6e17733
出典データセット
uspto-grants-1987_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04690941

反応ノート

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