Ammonium Hydroxide → HCID 13055817, 화합물

HRID 1155196노트

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HRID 1155196 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 13055817HCID 13055817, 화합물

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

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온도
0 °C

실험 절차

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 233°-225° C.). Recrystallization from methylene chloride gave cream colored prisms, mp 224°-225° C.

후처리

  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

출처 및 근거

ORD 기록
ord-28c4f8d3259743b2a75e0e22bee72426
출처 데이터셋
uspto-grants-1981_11
특허 번호
US04299971

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