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Triethylamine → HCID 19898936、化合物

HRID 1196545
ノート
印刷プレビュー

反応式

HRID 1196545 の反応式
[CH2:1]([N:8]([C:13]1[CH:18]=[CH:17][C:16]([CH:19]2[CH2:21][O:20]2)=[CH:15][CH:14]=1)[S:9]([CH3:12])(=[O:11])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:22][NH:23][CH2:24][CH2:25][N:26]1[N:35]=[CH:34][C:33]2[C:28](=[CH:29][CH:30]=[CH:31][CH:32]=2)[C:27]1=[O:36].C(N(CC)CC)C>C(O)(C)C>[CH2:1]([N:8]([C:13]1[CH:14]=[CH:15][C:16]([CH:19]([OH:20])[CH2:21][N:23]([CH2:24][CH2:25][N:26]2[N:35]=[CH:34][C:33]3[C:28](=[CH:29][CH:30]=[CH:31][CH:32]=3)[C:27]2=[O:36])[CH3:22])=[CH:17][CH:18]=1)[S:9]([CH3:12])(=[O:10])=[O:11])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 198989582-(2-(Methylamino)ethyl)phthalazin-1(2H)-oneHCID 54231897HCID 54231897、化合物

生成物 1

HCID 19898936HCID 19898936、化合物

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

2-{4-(N-Benzylmethanesulphonamido)phenyl]oxirane (1.5 g), N-methyl-2-(phthalazin-1-on-2-yl)ethylamine (1.4 g) and triethylamine (1.4 g) in isopropanol (50 ml) were stirred at reflux temperature for 5 hours. The solvent was evaporated, the residue dissolved in methylene chloride and washed three times with sodium carbonate solution and three times with brine. The organic layer was dried and evaporated to give an oil which was purified by column chromatography on silica, "Kieselgel 60" (Merck, Trade Mark), eluting with methylene chloride containing methanol (0% up to 2%). Combination and evaporation of the appropriate fractions gave a foam which was chromatographed a second time on silica, "Kieselgel 60" (Merck, Trade Mark), eluting with methyl isobutyl ketone (MIBK) containing acetone (0% up to 20%). The appropriate fractions were combined and evaporated then re-evaporated from diethyl ether to give the title compound as a foam, yield 450 mg.

後処理

  1. temperatureat reflux temperature for 5 hours
  2. customThe solvent was evaporated
  3. dissolutionthe residue dissolved in methylene chloride
  4. washwashed three times with sodium carbonate solution and three times with brine
  5. customThe organic layer was dried
  6. customevaporated
  7. customto give an oil which
  8. customwas purified by column chromatography on silica, "Kieselgel 60" (Merck, Trade Mark)
  9. washeluting with methylene chloride
  10. additioncontaining methanol (0% up to 2%)
  11. customCombination and evaporation of the appropriate fractions
  12. customgave a foam which
  13. customwas chromatographed a second time on silica, "Kieselgel 60" (Merck, Trade Mark)
  14. washeluting with methyl isobutyl ketone (MIBK)
  15. additioncontaining acetone (0% up to 20%)
  16. customevaporated
  17. customthen re-evaporated from diethyl ether

出典と根拠

ORDレコード
ord-72f4768b3a2b433580ed7bec69c2d8ba
出典データセット
uspto-grants-1992_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05114952

反応ノート

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