Hydrochloric Acid → HCID 178441131、化合物

HRID 260373ノート

反応式

HRID 260373 の反応式
[C:1]([C:5]1[CH:6]=[C:7]([CH:17]=[C:18]([C:21]([CH3:24])([CH3:23])[CH3:22])[C:19]=1[OH:20])[NH:8][C:9]1[CH:10]=[C:11]([CH:14]=[CH:15][CH:16]=1)[C:12]#[N:13])([CH3:4])([CH3:3])[CH3:2].[N-:25]=[N+:26]=[N-:27].[Na+].[Cl-].[NH4+].[Cl-].[Li+].Cl>CN(C)C=O>[C:1]([C:5]1[CH:6]=[C:7]([CH:17]=[C:18]([C:21]([CH3:24])([CH3:23])[CH3:22])[C:19]=1[OH:20])[NH:8][C:9]1[CH:10]=[C:11]([C:12]2[NH:27][N:26]=[N:25][N:13]=2)[CH:14]=[CH:15][CH:16]=1)([CH3:4])([CH3:3])[CH3:2]

参加物

7

反応物 5

HCID 313Hydrochloric AcidHCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 433294Lithium ChlorideHCID 224015743-(3,5-Di-t-butyl-4-hydroxyanilino)benzonitrile

生成物 1

HCID 178441131HCID 178441131、化合物収率 65.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
110 °C

実験手順

Eight g (0.025 mole) of 3-(3,5-di-t-butyl-4-hydroxyanilino)benzonitrile (from Example 27), 4.9 g (0.075 mole) of sodium azide, 4.0 g (0.075 mole) of ammonium chloride, 1.06 g (0.025 mole) of lithium chloride and 60 ml of N,N-dimethylformamide were combined under a nitrogen atmosphere and heated at 110° C. for 48 hours. The reaction mixture was poured into cold 6N hydrochloric acid and a gummy solid precipitated out. The supernatant was decanted off and the residue dissolved in ethanol. The ethanol solution was diluted with water and a pink solid was collected. This material was recrystallized from a mixture of ethanol and water to give 5.97 g of 5-[3-(3,5-di-t-butyl-4-hydroxyanilino)phenyl]tetrazole, m.p. 231°-233° C. Analysis: Calculated for C21H27N5O: % C, 69.0; % H, 7.4; % N, 19.2; Found: % C, 68.4; % H, 7.6; % N, 18.8.

後処理

  1. customa gummy solid precipitated out
  2. customThe supernatant was decanted off
  3. dissolutionthe residue dissolved in ethanol
  4. additionThe ethanol solution was diluted with water
  5. customa pink solid was collected
  6. customThis material was recrystallized from a mixture of ethanol and water

出典と根拠

ORDレコード
ord-3dc86c6f154743c3bb9f9c31ff83eead
出典データセット
uspto-grants-1996_06
特許番号
US05527824

反応ノート

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