N-Bromoacetamide → s-Triazolo(5,1-a)isoquinoline, 2-phenyl-

HRID 1733136

反応式

HRID 1733136 の反応式
[C:1]1([C:7]2[N:19]=[C:10]3[C:11]4[C:16]([CH2:17][CH2:18][N:9]3[N:8]=2)=[CH:15][CH:14]=[CH:13][CH:12]=4)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.BrNC(=O)C>C(Cl)(Cl)(Cl)Cl>[C:1]1([C:7]2[N:19]=[C:10]3[C:11]4[C:16]([CH:17]=[CH:18][N:9]3[N:8]=2)=[CH:15][CH:14]=[CH:13][CH:12]=4)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

4

反応物 2

HCID 4353N-BromoacetamideHCID 134397s-Triazolo(5,1-a)isoquinoline, 5,6-dihydro-2-phenyl-

生成物 1

HCID 169678s-Triazolo(5,1-a)isoquinoline, 2-phenyl-収率 79%

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

実験手順

A mixture of 0.5 g. (0.002 mole) of 2-phenyl-5,6-dihydro-s-triazolo[5,1-a]isoquinoline and 0.28 g. (0.002 mole) of N-bromoacetamide in 10 ml. of carbon tetrachloride is refluxed for 5 hours. The crystalline precipitate which forms is filtered and dissolved in methylene chloride. The resulting solution is washed with sodium bicarbonate, then the solvent is evaporated off and the obtained residue recrystallized from ethyl acetate. Yield 79%.

後処理

  1. additionA mixture of 0.5 g
  2. filtrationThe crystalline precipitate which forms is filtered
  3. dissolutiondissolved in methylene chloride
  4. washThe resulting solution is washed with sodium bicarbonate
  5. customthe solvent is evaporated off
  6. customthe obtained residue recrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-f346b66ca0f74710856de359163131a4
出典データセット
uspto-grants-1980_12
特許番号
USRE030456

関連ノート

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