Allyl bromide → HCID 12941265、化合物

HRID 1277424ノート

反応式

HRID 1277424 の反応式
[CH:1]1([N:7]2[C:11]([CH2:12][CH2:13][CH2:14][O:15][C:16]3[CH:17]=[C:18]4[C:23](=[CH:24][CH:25]=3)[NH:22][C:21](=[O:26])[CH:20]=[CH:19]4)=[N:10][N:9]=[N:8]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[H-].[Na+].[CH2:29](Br)[CH:30]=[CH2:31]>CN(C)C=O>[CH2:31]([N:22]1[C:23]2[C:18](=[CH:17][C:16]([O:15][CH2:14][CH2:13][CH2:12][C:11]3[N:7]([CH:1]4[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]4)[N:8]=[N:9][N:10]=3)=[CH:25][CH:24]=2)[CH:19]=[CH:20][C:21]1=[O:26])[CH:30]=[CH2:29]

参加物

5

反応物 3

HCID 7841Allyl bromideHCID 24758Sodium hydrideHCID 130210946-[3-(1-Cyclohexyl-1H-tetrazol-5-yl) propoxy]-2(1H)-quinolinone

生成物 1

HCID 12941265HCID 12941265、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Into 50 ml of dimethylformamide, 1.8 g of 6-[3-(1-cyclohexyltetrazol-5-yl)propoxy]carbostyril is dissolved, then 0.15 g of NaH is added under stirring for 30 minutes by ice-cooling the outside of the reaction vessel. Into the reaction mixture, 0.52 ml of allyl bromide is added dropwise and stirred at a room temperature for 2 hours. The reaction mixture is then concentrated and the residue is extracted with chloroform, washed with water and dried with Na2SO4. After removal of the drying agent by filtration, the mother liquor is concentrated and the residue is dissolved in chloroform. The chloroform solution is washed with water and then concentrated. The residue thus obtained is purified by a silica gel column chromatography [eluent: chloroform-methanol (50:1)]. The eluted solution is concentrated and the residue is recrystallized from chloroform-petroleum ether to obtain 1.2 g of 1-allyl-6-[3-(1-cyclohexyltetrazol-5-yl)propoxy]carbostyril in the form ofcolorless needle-like crystals. Melting point: 102°-103.5° C.

後処理

  1. temperaturecooling the outside of the reaction vessel
  2. stirringstirred at a room temperature for 2 hours
  3. concentrationThe reaction mixture is then concentrated
  4. extractionthe residue is extracted with chloroform
  5. washwashed with water
  6. dry with materialdried with Na2SO4
  7. customAfter removal of the drying agent
  8. filtrationby filtration
  9. concentrationthe mother liquor is concentrated
  10. dissolutionthe residue is dissolved in chloroform
  11. washThe chloroform solution is washed with water
  12. concentrationconcentrated
  13. customThe residue thus obtained
  14. customis purified by a silica gel column chromatography [eluent: chloroform-methanol (50:1)]
  15. concentrationThe eluted solution is concentrated
  16. customthe residue is recrystallized from chloroform-petroleum ether

出典と根拠

ORDレコード
ord-0217019033464099a1eda23ef850c3d7
出典データセット
uspto-grants-1981_07
特許番号
US04277479

反応ノート

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