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Benzaldehyde → HCID 19838485、化合物

HRID 476755
ノート
印刷プレビュー

反応式

HRID 476755 の反応式
Cl.[NH2:2][CH:3]1[CH2:15][C:14]2[C:6](=[CH:7][C:8]3[CH2:12][CH2:11][O:10][C:9]=3[CH:13]=2)[CH2:5][CH2:4]1.[CH:16](=O)[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>C1C=CC=CC=1>[CH2:16]([NH:2][CH:3]1[CH2:15][C:14]2[C:6](=[CH:7][C:8]3[CH2:12][CH2:11][O:10][C:9]=3[CH:13]=2)[CH2:5][CH2:4]1)[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=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 240BenzaldehydeHCID 19838440HCID 19838440、化合物

生成物 1

HCID 19838485HCID 19838485、化合物

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

45 g of the compound of Example 2, 25.4 g of benzaldehyde and 300 ml of benzene are brought to reflux, removing the water formed. The mixture is evaporated to dryness, the residue is taken up with 300 ml of ethanol and 9 g of sodium borohydride are added portionwise, keeping the temperature at approximately 18° C. After one night at room temperature, the ethanol is removed under vacuum and the residue taken up with dilute hydrochloric acid solution. The acid phase is alkalinized and then extracted with ethyl ether. After evaporation of the solvent, the oil obtained is purified on a silica column using a mixture of methylene chloride and methanol (95:5 V/V) as elution solvent.

後処理

  1. temperatureto reflux
  2. customremoving the water
  3. customformed
  4. customThe mixture is evaporated to dryness
  5. additionare added portionwise
  6. customat approximately 18° C
  7. waitAfter one night at room temperature
  8. customthe ethanol is removed under vacuum
  9. extractionextracted with ethyl ether
  10. customAfter evaporation of the solvent
  11. customthe oil obtained
  12. customis purified on a silica column
  13. additiona mixture of methylene chloride and methanol (95:5 V/V)
  14. washas elution solvent

出典と根拠

ORDレコード
ord-366b1096f35f453da4c822907905d8d2
出典データセット
uspto-grants-1989_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04885373

反応ノート

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