Ammonium Hydroxide → HCID 13055817、化合物

HRID 1389032ノート

反応式

HRID 1389032 の反応式
[C:1]1([C:7]2[C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=3[C:11]3=[N:18][NH:19][N:20]=[C:10]3[CH2:9][N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[N+:21]([O-])([O-:23])=[O:22].[K+].[OH-].[NH4+]>S(=O)(=O)(O)O>[N+:21]([C:5]1[CH:6]=[C:1]([C:7]2[C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=3[C:11]3=[N:18][NH:19][N:20]=[C:10]3[CH2:9][N:8]=2)[CH:2]=[CH:3][CH:4]=1)([O-:23])=[O:22]

参加物

5

反応物 3

HCID 14923Ammonium HydroxideHCID 24434Potassium NitrateHCID 30604501,2,3-Triazolo(4,5-d)(2)benzazepine, 2,4-dihydro-6-phenyl-

生成物 1

HCID 13055817HCID 13055817、化合物

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

反応条件

温度
0 °C

実験手順

A mixture of 1.6 g (4.5 mmole) of the methanesulfonate salt of 6-phenyl-2H, 4H-[1,2,3]triazolo[4,5-d][2]benzazepine, 8.6 g of potassium nitrate, and 20 ml of sulfuric acid was stirred at 0° C. for 3.5 hr. The mixture was poured over ice, basified with ammonium hydroxide and extracted with methylene chloride. The methylene chloride solution was dried with anhydrous sodium sulfate and concentrated at reduced pressure. The residue was triturated with ether to give tan crystals (mp 223°-225° C.). Recrystallization from methylene chloride gave cream colored prisms, mp 224°-225° C.

後処理

  1. additionThe mixture was poured over ice
  2. extractionextracted with methylene chloride
  3. dry with materialThe methylene chloride solution was dried with anhydrous sodium sulfate
  4. concentrationconcentrated at reduced pressure
  5. customThe residue was triturated with ether

出典と根拠

ORDレコード
ord-1b20af14f4a244679041ffabfe7f9242
出典データセット
uspto-grants-1981_01
特許番号
US04243589

反応ノート

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